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_4342148
_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_absolute_configuration ad
_chemical_formula_moiety         'C44 H68 Ga2 N6, C6 H14'
_chemical_formula_sum            'C50 H82 Ga2 N6'
_chemical_formula_weight         906.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-17
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.58929(15)
_cell_length_b                   18.9059(2)
_cell_length_c                   20.0649(2)
_cell_measurement_reflns_used    18780
_cell_measurement_temperature    151.0
_cell_measurement_theta_max      29.3071
_cell_measurement_theta_min      2.7385
_cell_volume                     5155.03(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      151.0
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_details
;
  1 omega  -90.00  -60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  179.0000  -90.0000 30

  2 omega  -14.00   27.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1366   92.0000  -84.0000 41

  3 omega  -17.00   23.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1366  -37.0000 -180.0000 40

  4 omega  -10.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1366    0.0000   60.0000 101

  5 omega  -90.00    8.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  -37.0000   90.0000 98

  6 omega  -53.00  -28.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1366  -37.0000   30.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0371255000
_diffrn_orient_matrix_UB_12      -0.0095909000
_diffrn_orient_matrix_UB_13      0.0231461000
_diffrn_orient_matrix_UB_21      -0.0304486000
_diffrn_orient_matrix_UB_22      0.0114411000
_diffrn_orient_matrix_UB_23      0.0266121000
_diffrn_orient_matrix_UB_31      -0.0204633000
_diffrn_orient_matrix_UB_32      -0.0344196000
_diffrn_orient_matrix_UB_33      0.0023960000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36228
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.37
_diffrn_reflns_theta_min         2.74
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
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    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(7)
_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     546
_refine_ls_number_reflns         12217
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0342P)^2^+2.1978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                10857
_reflns_number_total             12217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5029096_si_002.cif
_cod_data_source_block           compound_16
_cod_depositor_comments
'Adding full bibliography for 4342142--4342150.cif.'
_cod_original_cell_volume        5155.05(10)
_cod_database_code               4342148
_chemical_oxdiff_formula         C40H40N8GA2
_chemical_oxdiff_usercomment     'AT 150K'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H27 of C27, {H46A,H46B} of C46, {H48A,H48B} of C48, {H47A,H47B} of C47,
  {H49A,H49B} of C49, H3 of N3, H13 of C13, H15 of C15, H18 of C18, H23 of C23,
  H30 of C30, H36 of C36, H39 of C39, H35 of C35, H42 of C42, H37 of C37, H12
  of C12, H25 of C25, H11 of C11, H24 of C24
 At 1.5 times of:
  {H16A,H16B,H16C} of C16, {H31A,H31B,H31C} of C31, {H19A,H19B,H19C} of C19,
  {H28A,H28B,H28C} of C28, {H40A,H40B,H40C} of C40, {H45A,H45B,H45C} of C45,
  {H50A,H50B,H50C} of C50, {H20A,H20B,H20C} of C20, {H5A,H5B,H5C} of C5, {H41A,
  H41B,H41C} of C41, {H29A,H29B,H29C} of C29, {H8A,H8B,H8C} of C8, {H44A,H44B,
  H44C} of C44, {H43A,H43B,H43C} of C43, {H17A,H17B,H17C} of C17, {H32A,H32B,
  H32C} of C32, {H6A,H6B,H6C} of C6, {H7A,H7B,H7C} of C7, {H4A,H4B,H4C} of C4
2. Restrained distances
 C46-C47
 1.72 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C42(H42), C39(H39), C30(H30), C15(H15), C18(H18), C27(H27)
3.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C49(H49A,H49B), C48(H48A,H48B), C46(H46A,H46B)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C37(H37), C12(H12), C35(H35), C36(H36), C23(H23), C24(H24), C11(H11),
 C25(H25), C13(H13)
3.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C8(H8A,H8B,
 H8C), C29(H29A,H29B,H29C), C41(H41A,H41B,H41C), C4(H4A,H4B,H4C), C7(H7A,H7B,
 H7C), C6(H6A,H6B,H6C), C32(H32A,H32B,H32C), C20(H20A,H20B,H20C), C5(H5A,H5B,
 H5C), C16(H16A,H16B,H16C), C31(H31A,H31B,H31C), C19(H19A,H19B,H19C), C28(H28A,
 H28B,H28C), C40(H40A,H40B,H40C), C45(H45A,H45B,H45C), C50(H50A,H50B,H50C)
;