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_4342146
_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         'C59 H74 Ga2 N6'
_chemical_formula_sum            'C59 H74 Ga2 N6'
_chemical_formula_weight         1006.68
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                97.568(7)
_cell_angle_beta                 101.971(6)
_cell_angle_gamma                111.337(7)
_cell_formula_units_Z            2
_cell_length_a                   11.8841(7)
_cell_length_b                   13.1349(11)
_cell_length_c                   19.4386(16)
_cell_measurement_reflns_used    3262
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      24.0060
_cell_measurement_theta_min      3.6810
_cell_volume                     2692.4(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      150.00(14)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0141810000
_diffrn_orient_matrix_UB_12      -0.0568198000
_diffrn_orient_matrix_UB_13      0.0015965000
_diffrn_orient_matrix_UB_21      0.0636542000
_diffrn_orient_matrix_UB_22      0.0091765000
_diffrn_orient_matrix_UB_23      0.0031302000
_diffrn_orient_matrix_UB_31      0.0138860000
_diffrn_orient_matrix_UB_32      0.0152178000
_diffrn_orient_matrix_UB_33      0.0381421000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1046
_diffrn_reflns_av_unetI/netI     0.1463
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22225
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.68
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.283
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         9394
_refine_ls_number_restraints     450
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1923
_reflns_number_gt                5683
_reflns_number_total             9394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5029096_si_002.cif
_cod_data_source_block           compound_14
_cod_depositor_comments
'Adding full bibliography for 4342142--4342150.cif.'
_cod_original_cell_volume        2692.4(3)
_cod_database_code               4342146
_chemical_oxdiff_formula         'C40 H40 Ga4 N8'
_chemical_oxdiff_usercomment     'AT 150 K, COLORLESS, BLOCK'
_reflns_odcompleteness_completeness 99.17
_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 C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C66-C50
 1.54 with sigma of 0.02
 C57A-C23
 1.541 with sigma of 0.02
 C72-C23
 1.53 with sigma of 0.02
 C72A-C23
 1.58 with sigma of 0.02
3. Rigid bond restraints
 C1, C50
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C53, C62
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C7) = Uanis(C2) = Uanis(C1) = Uanis(C66)
Uanis(C23) = Uanis(C57) = Uanis(C57A) = Uanis(C72) = Uanis(C72A)
Uanis(C39) = Uanis(C67) = Uanis(C54)
Uanis(C15) = Uanis(C26)
Uanis(C34) = Uanis(C55)
Uanis(C28) = Uanis(C69) = Uanis(C62) = Uanis(C29)
5. Others
 Sof(H50A)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C7)=Sof(H7A)=Sof(H7B)=
 Sof(H7C)=1-FVAR(1)
 Sof(H50)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(H2C)=FVAR(1)
 Sof(H23A)=Sof(C57A)=Sof(H57D)=Sof(H57E)=Sof(H57F)=Sof(C72A)=Sof(H72D)=
 Sof(H72E)=Sof(H72F)=1-FVAR(2)
 Sof(H23)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C72)=Sof(H72A)=Sof(H72B)=
 Sof(H72C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C20(H20), C23(H23), C23(H23A), C34(H34), C39(H39), C44(H44), C50(H50),
 C50(H50A)
6.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C6(H6), N9(H9), C11(H11), C12(H12), C16(H16), C17(H17), C18(H18),
 C22(H22), C24(H24), C40(H40), C41(H41), C42(H42), C45(H45), C46(H46), C49(H49),
  C51(H51), C52(H52), C53(H53), C56(H56), C58(H58), C59(H59), C60(H60),
 C61(H61), C62(H62), C69(H69)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C43(H43A,H43B,H43C), C48(H48A,H48B,H48C), C54(H54A,
 H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C66(H66A,H66B,H66C),
 C67(H67A,H67B,H67C), C72(H72A,H72B,H72C), C1(H1A,H1B,H1C), C7(H7A,H7B,H7C),
 C2(H2A,H2B,H2C), C57A(H57D,H57E,H57F), C72A(H72D,H72E,H72F)
;