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_4342143
_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         'C57 H56 Ga4 N8, C7 H8'
_chemical_formula_sum            'C64 H64 Ga4 N8'
_chemical_formula_weight         1224.11
_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             2014-10-21
_audit_creation_method
;
  Olex2 1.2
  (compiled Oct 26 2012 17:06:22, GUI svn.r4371)
;
_cell_angle_alpha                93.330(2)
_cell_angle_beta                 113.944(3)
_cell_angle_gamma                101.566(3)
_cell_formula_units_Z            2
_cell_length_a                   14.1348(5)
_cell_length_b                   14.1580(4)
_cell_length_c                   16.4427(5)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      29.1767
_cell_measurement_theta_min      3.7094
_cell_volume                     2910.33(18)
_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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      149(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_details
;
  1 omega  -42.00   51.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   37.0000 -120.0000 93

  2 omega  -23.00   25.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -99.0000 -150.0000 48

  3 omega  -85.00   11.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -77.0000  -30.0000 96

  4 omega  -90.00    6.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -37.0000   60.0000 96

  5 omega  -86.00    4.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -57.0000 -150.0000 90

  6 omega  -93.00  -43.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397 -178.0000 -150.0000 50

  7 omega   32.00   96.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0585 -178.0000  150.0000 64
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0466835000
_diffrn_orient_matrix_UB_12      0.0198117000
_diffrn_orient_matrix_UB_13      -0.0057959000
_diffrn_orient_matrix_UB_21      -0.0253082000
_diffrn_orient_matrix_UB_22      0.0341585000
_diffrn_orient_matrix_UB_23      -0.0249142000
_diffrn_orient_matrix_UB_31      0.0197056000
_diffrn_orient_matrix_UB_32      0.0334772000
_diffrn_orient_matrix_UB_33      0.0403591000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31236
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         3.72
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.878
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75514
_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    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         13415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0320P)^2^+1.3632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                10796
_reflns_number_total             13415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5029096_si_002.cif
_cod_data_source_block           compound_6
_cod_depositor_comments
'Adding full bibliography for 4342142--4342150.cif.'
_cod_original_cell_volume        2910.32(16)
_cod_database_code               4342143
_chemical_oxdiff_formula         'C40 H40 Ga4 N8'
_chemical_oxdiff_usercomment     '150 K, COLORLESS, BLOCK, .42 .26 .22'
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H62 of C62, H63 of C63, H61 of C61, H64 of C64, H60 of C60, H43 of C43, H42
  of C42, H44 of C44, H36 of C36, H31 of C31, H13 of C13, H30 of C30, H37 of
  C37, H32 of C32, H54 of C54, H56 of C56, H45 of C45, H11 of C11, H21 of C21,
  H33 of C33, H17 of C17, H23 of C23, H51 of C51, H18 of C18, H53 of C53, H12
  of C12, H41 of C41, H50 of C50, H15 of C15, H49 of C49, H38 of C38, H27 of
  C27, H39 of C39, H20 of C20, H29 of C29, {H6A,H6B,H6C} of C6, H24 of C24, H35
  of C35, H26 of C26, H47 of C47, H19 of C19, H25 of C25, H57 of C57, H48 of
  C48, H55 of C55, H14 of C14, {H9A,H9B,H9C} of C9
 At 1.5 times of:
  {H5A,H5B,H5C} of C5, {H58A,H58B,H58C} of C58, {H8A,H8B,H8C} of C8, {H7A,H7B,
  H7C} of C7
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C21(H21), C33(H33), C17(H17), C23(H23), C51(H51), C18(H18),
 C53(H53), C12(H12), C41(H41), C50(H50), C15(H15), C49(H49), C38(H38), C27(H27),
  C39(H39), C20(H20), C29(H29), C24(H24), C35(H35), C26(H26), C47(H47),
 C19(H19), C25(H25), C57(H57), C48(H48), C55(H55), C14(H14), C45(H45), C56(H56),
  C54(H54), C32(H32), C37(H37), C30(H30), C13(H13), C31(H31), C36(H36),
 C44(H44), C42(H42), C43(H43), C60(H60), C64(H64), C61(H61), C63(H63), C62(H62)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C8(H8A,
 H8B,H8C), C58(H58A,H58B,H58C)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'