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_4342145
_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         '2(C37 H48 Ga4 N8), C7 H8'
_chemical_formula_sum            'C81 H104 Ga8 N16'
_chemical_formula_weight         1859.56
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-20
_audit_creation_method
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Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
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_cell_length_a                   13.0751(6)
_cell_length_b                   13.6722(6)
_cell_length_c                   14.7834(6)
_cell_measurement_reflns_used    4487
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      29.1145
_cell_measurement_theta_min      3.5679
_cell_volume                     2114.07(19)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_details
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  1 omega  -74.00    4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -57.0000    0.0000 78

  2 omega  -19.00   25.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -99.0000  -90.0000 44

  3 omega  -81.00  -43.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397 -178.0000 -150.0000 38

  4 omega  -90.00    5.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -37.0000 -180.0000 95

  5 omega  -25.00   11.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -99.0000  150.0000 36

  6 omega  -81.00   23.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -19.0000   60.0000 104

  7 omega  -57.00   30.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   95.0000  138.0000 87
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_diffrn_measurement_device_type  'Xcalibur, Eos'
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_diffrn_orient_matrix_UB_33      -0.0190428000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_Laue_measured_fraction_full 0.992
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_diffrn_reflns_limit_h_min       -17
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_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19783
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.179
_diffrn_reflns_theta_min         3.575
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.560
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87763
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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.
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_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
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_refine_diff_density_max         1.301
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_refine_ls_number_reflns         9648
_refine_ls_number_restraints     0
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+1.7804P] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5029096_si_002.cif
_cod_data_source_block           compound_11
_cod_depositor_comments
'Adding full bibliography for 4342142--4342150.cif.'
_cod_database_code               4342145
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C40 H40 Ga4 N8'
_chemical_oxdiff_usercomment     'AT 140 K, COLORLESS, BLOCK'
_reflns_odcompleteness_completeness 99.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(C40) = Uiso(C41)
Uiso(C37) = Uiso(C38)
3. Others
 Fixed Sof: C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C37(0.5) C42(0.5) H42(0.5)
 C41(0.5) H41(0.5) C40(0.5) H40(0.5) C39(0.5) H39(0.5) C38(0.5) H38(0.5)
4.a Free rotating group:
 C36(C37,C42,C41,C40,C39,C38)
4.b Aromatic/amide H refined with riding coordinates:
 N8(H8), C34(H34), C33(H33), C35(H35), C31(H31), C19(H19), C32(H32), C29(H29),
 C16(H16), C23(H23), C14(H14), C15(H15), C20(H20), C1A(H1A), C25(H25), C28(H28),
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 C39(H39), C38(H38)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C24(H24A,H24B,H24C), C5(H5A,H5B,H5C), C43(H43A,H43B,H43C),
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C),
 C36(H36A,H36B,H36C)
;
_olex2_submission_special_instructions 'No special instructions were received'