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_4342144
_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         'C80 H100 Ga4 N8, 2(C7 H8)'
_chemical_formula_sum            'C94 H116 Ga4 N8'
_chemical_formula_weight         1636.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90.00
_cell_angle_beta                 98.561(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.0426(12)
_cell_length_b                   10.3599(4)
_cell_length_c                   31.2885(17)
_cell_measurement_reflns_used    6973
_cell_measurement_temperature    120.1(2)
_cell_measurement_theta_max      29.2964
_cell_measurement_theta_min      2.5921
_cell_volume                     9309.1(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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
;
SHELXH, 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      120.1(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9861
_diffrn_measurement_details
;
  1 omega   64.00   95.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022  179.0000   90.0000 31

  2 omega  -43.00   72.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022    0.0000  -90.0000 115

  3 omega   20.00   89.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022   77.0000   60.0000 69

  4 omega  -43.00   55.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1835   37.0000 -180.0000 98

  5 omega  -11.00   16.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9022   77.0000  -90.0000 27
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0208035000
_diffrn_orient_matrix_UB_12      0.0299957000
_diffrn_orient_matrix_UB_13      -0.0042153000
_diffrn_orient_matrix_UB_21      -0.0067618000
_diffrn_orient_matrix_UB_22      -0.0103456000
_diffrn_orient_matrix_UB_23      -0.0224675000
_diffrn_orient_matrix_UB_31      -0.0114465000
_diffrn_orient_matrix_UB_32      0.0606925000
_diffrn_orient_matrix_UB_33      -0.0017469000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            33107
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.36
_diffrn_reflns_theta_min         2.60
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.191
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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       prism
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0470P)^2^+0.5165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1049
_reflns_number_gt                6217
_reflns_number_total             8203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5029096_si_002.cif
_cod_data_source_block           compound_8
_cod_depositor_comments
'Adding full bibliography for 4342142--4342150.cif.'
_cod_database_code               4342144
_chemical_oxdiff_formula         'C40 H60 N8 GA4'
_chemical_oxdiff_usercomment     'AT 120K'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H27 of C27, H26 of C26, H7 of C7, H25 of C25, H31 of C31, H15 of C15, H17
  of C17, H13 of C13, H42 of C42, H46 of C46, H43 of C43, H8 of C8, H9 of C9,
  H28 of C28, H38 of C38, H14 of C14, H6 of C6, H20 of C20, H33 of C33, H35 of
  C35, H24 of C24, H45 of C45, H44 of C44, H10 of C10, H32 of C32
 At 1.5 times of:
  {H19A,H19B,H19C} of C19, {H37A,H37B,H37C} of C37, {H21A,H21B,H21C} of C21,
  {H39A,H39B,H39C} of C39, {H36A,H36B,H36C} of C36, {H40A,H40B,H40C} of C40,
  {H3A,H3B,H3C} of C3, {H18A,H18B,H18C} of C18, {H1A,H1B,H1C} of C1, {H47A,H47B,
  H47C} of C47, {H22A,H22B,H22C} of C22
2.a Ternary CH refined with riding coordinates:
 C38(H38), C20(H20), C35(H35), C17(H17)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C33(H33), C24(H24), C10(H10), C32(H32), C27(H27), C26(H26),
 C7(H7), C25(H25), C31(H31), C15(H15), C13(H13), C28(H28), C9(H9), C8(H8),
 C43(H43), C46(H46), C42(H42), C44(H44), C45(H45)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C18(H18A,H18B,H18C), C3(H3A,H3B,H3C),
 C40(H40A,H40B,H40C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C21(H21A,H21B,
 H21C), C37(H37A,H37B,H37C), C19(H19A,H19B,H19C), C47(H47A,H47B,H47C)
;