 
data_1b
 
_audit_creation_method            SHELXL-2014/6
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C8 H25 Al0.84 Ga1.16 N3' 
_chemical_formula_weight          266.85

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al'  'Al'   0.0645   0.0514
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ga'  'Ga'   0.2307   1.6083
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            19
_space_group_name_H-M_alt         'P 21 21 21'
_space_group_name_Hall            'P 2ac 2ab'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 
_cell_length_a                    6.2256(8)
_cell_length_b                    12.9136(15)
_cell_length_c                    17.444(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1402.4(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.264          
_exptl_crystal_F_000              564
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.400
_exptl_crystal_size_mid           0.300
_exptl_crystal_size_min           0.200
_exptl_absorpt_coefficient_mu     2.286
_shelx_estimated_absorpt_T_min    0.462
_shelx_estimated_absorpt_T_max    0.658
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             13109
_diffrn_reflns_av_unetI/netI      0.0199
_diffrn_reflns_av_R_equivalents   0.0293
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          1.962
_diffrn_reflns_theta_max          25.040
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  0.977
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   0.977
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  0.974
_reflns_number_total              2482
_reflns_number_gt                 2334
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.698
_reflns_Friedel_fraction_max      1.000
_reflns_Friedel_fraction_full     0.971
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0271P)²+0.2580P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.435(15)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          2482
_refine_ls_number_parameters      142
_refine_ls_number_restraints      8
_refine_ls_R_factor_all           0.0237
_refine_ls_R_factor_gt            0.0204
_refine_ls_wR_factor_ref          0.0504
_refine_ls_wR_factor_gt           0.0490
_refine_ls_goodness_of_fit_ref    1.044
_refine_ls_restrained_S_all       1.044
_refine_ls_shift/su_max           0.017
_refine_ls_shift/su_mean          0.002
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Al1 Al 0.2398(12) 0.4290(9) 0.0350(5) 0.0260(8) Uani 0.844(2) 1 d D . P A 1
Ga1 Ga 0.254(3) 0.4339(18) 0.0443(11) 0.0260(8) Uani 0.156(2) 1 d D . P A 2
H1' H 0.014(3) 0.440(2) 0.0373(16) 0.031 Uiso 1 1 d D U . . .
H2' H 0.366(4) 0.3612(19) -0.0094(15) 0.031 Uiso 1 1 d D U . . .
Ga2 Ga 0.20888(6) 0.61248(3) 0.17694(2) 0.04468(13) Uani 1 1 d D . . . .
H3' H 0.357(4) 0.620(2) 0.2395(14) 0.054 Uiso 1 1 d D U . . .
H4' H 0.154(4) 0.7110(17) 0.1457(17) 0.054 Uiso 1 1 d D U . . .
H5' H 0.027(4) 0.551(2) 0.1970(16) 0.054 Uiso 1 1 d D U . . .
N1 N 0.3043(4) 0.55591(18) -0.04642(13) 0.0375(5) Uani 1 1 d . . . . .
N2 N 0.4030(4) 0.52312(18) 0.10749(14) 0.0314(5) Uani 1 1 d . . . . .
N3 N 0.2682(4) 0.32177(17) 0.13327(12) 0.0328(5) Uani 1 1 d . . . . .
C1 C 0.1045(6) 0.5938(3) -0.0822(2) 0.0544(9) Uani 1 1 d . . . . .
H1A H 0.1380 0.6511 -0.1170 0.082 Uiso 1 1 calc R U . . .
H1B H 0.0059 0.6180 -0.0422 0.082 Uiso 1 1 calc R U . . .
H1C H 0.0369 0.5375 -0.1110 0.082 Uiso 1 1 calc R U . . .
C2 C 0.4517(7) 0.5194(3) -0.1073(2) 0.0579(10) Uani 1 1 d . . . . .
H2A H 0.4782 0.5757 -0.1437 0.087 Uiso 1 1 calc R U . . .
H2B H 0.3865 0.4607 -0.1342 0.087 Uiso 1 1 calc R U . . .
H2C H 0.5879 0.4976 -0.0842 0.087 Uiso 1 1 calc R U . . .
C3 C 0.4086(5) 0.6396(2) -0.00213(18) 0.0415(7) Uani 1 1 d . . . . .
H3A H 0.2980 0.6861 0.0197 0.050 Uiso 1 1 calc R U . . .
H3B H 0.5020 0.6811 -0.0363 0.050 Uiso 1 1 calc R U . . .
C4 C 0.5411(5) 0.5931(3) 0.06152(18) 0.0419(7) Uani 1 1 d . . . . .
H4A H 0.6631 0.5537 0.0397 0.050 Uiso 1 1 calc R U . . .
H4B H 0.5996 0.6487 0.0945 0.050 Uiso 1 1 calc R U . . .
C5 C 0.5383(5) 0.4558(3) 0.15634(18) 0.0406(8) Uani 1 1 d . . . . .
H5A H 0.6099 0.4976 0.1964 0.049 Uiso 1 1 calc R U . . .
H5B H 0.6504 0.4219 0.1249 0.049 Uiso 1 1 calc R U . . .
C6 C 0.3965(5) 0.3749(2) 0.19306(15) 0.0377(7) Uani 1 1 d . . . . .
H6A H 0.4863 0.3238 0.2207 0.045 Uiso 1 1 calc R U . . .
H6B H 0.2994 0.4082 0.2306 0.045 Uiso 1 1 calc R U . . .
C7 C 0.0556(6) 0.2903(3) 0.16437(19) 0.0485(8) Uani 1 1 d . . . . .
H7A H 0.0765 0.2429 0.2076 0.073 Uiso 1 1 calc R U . . .
H7B H -0.0273 0.2555 0.1242 0.073 Uiso 1 1 calc R U . . .
H7C H -0.0224 0.3518 0.1818 0.073 Uiso 1 1 calc R U . . .
C8 C 0.3810(6) 0.2271(2) 0.1066(2) 0.0518(9) Uani 1 1 d . . . . .
H8A H 0.3847 0.1761 0.1482 0.078 Uiso 1 1 calc R U . . .
H8B H 0.5281 0.2449 0.0916 0.078 Uiso 1 1 calc R U . . .
H8C H 0.3046 0.1979 0.0626 0.078 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Al1 N2 2.027(9) . ?
Al1 N1 2.205(12) . ?
Al1 N3 2.211(11) . ?
Al1 H1' 1.41(2) . ?
Al1 H2' 1.41(2) . ?
Ga1 N2 1.85(2) . ?
Ga1 N3 2.12(2) . ?
Ga1 N1 2.25(2) . ?
Ga1 H1' 1.50(3) . ?
Ga1 H2' 1.50(2) . ?
Ga2 N2 2.064(2) . ?
Ga2 H3' 1.43(2) . ?
Ga2 H4' 1.43(2) . ?
Ga2 H5' 1.43(2) . ?
N1 C1 1.475(4) . ?
N1 C3 1.479(4) . ?
N1 C2 1.480(4) . ?
N2 C5 1.480(4) . ?
N2 C4 1.482(4) . ?
N3 C6 1.482(4) . ?
N3 C8 1.484(4) . ?
N3 C7 1.487(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.508(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.509(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N2 Al1 N1 82.3(4) . . ?
N2 Al1 N3 81.5(3) . . ?
N1 Al1 N3 161.9(4) . . ?
N2 Al1 H1' 114.8(12) . . ?
N1 Al1 H1' 97.0(13) . . ?
N3 Al1 H1' 97.1(13) . . ?
N2 Al1 H2' 115.9(12) . . ?
N1 Al1 H2' 90.4(12) . . ?
N3 Al1 H2' 89.5(12) . . ?
H1' Al1 H2' 129.4(17) . . ?
N2 Ga1 N3 88.2(8) . . ?
N2 Ga1 N1 85.0(10) . . ?
N3 Ga1 N1 169.5(9) . . ?
N2 Ga1 H1' 121.0(15) . . ?
N3 Ga1 H1' 98.0(16) . . ?
N1 Ga1 H1' 92.4(15) . . ?
N2 Ga1 H2' 122.0(14) . . ?
N3 Ga1 H2' 90.6(15) . . ?
N1 Ga1 H2' 86.3(14) . . ?
H1' Ga1 H2' 117(2) . . ?
N2 Ga2 H3' 96.0(13) . . ?
N2 Ga2 H4' 114.5(13) . . ?
H3' Ga2 H4' 112.9(12) . . ?
N2 Ga2 H5' 107.2(13) . . ?
H3' Ga2 H5' 111.1(11) . . ?
H4' Ga2 H5' 113.8(12) . . ?
C1 N1 C3 110.4(2) . . ?
C1 N1 C2 109.0(3) . . ?
C3 N1 C2 109.6(3) . . ?
C1 N1 Al1 111.4(3) . . ?
C3 N1 Al1 106.6(3) . . ?
C2 N1 Al1 109.8(3) . . ?
C1 N1 Ga1 114.3(4) . . ?
C3 N1 Ga1 101.8(5) . . ?
C2 N1 Ga1 111.5(4) . . ?
C5 N2 C4 109.9(2) . . ?
C5 N2 Ga1 105.3(7) . . ?
C4 N2 Ga1 110.4(7) . . ?
C5 N2 Al1 107.0(3) . . ?
C4 N2 Al1 108.6(4) . . ?
C5 N2 Ga2 108.88(18) . . ?
C4 N2 Ga2 108.45(18) . . ?
Ga1 N2 Ga2 113.9(4) . . ?
Al1 N2 Ga2 114.1(2) . . ?
C6 N3 C8 110.3(2) . . ?
C6 N3 C7 110.5(2) . . ?
C8 N3 C7 108.1(3) . . ?
C6 N3 Ga1 102.8(6) . . ?
C8 N3 Ga1 110.6(4) . . ?
C7 N3 Ga1 114.6(5) . . ?
C6 N3 Al1 107.4(3) . . ?
C8 N3 Al1 108.1(3) . . ?
C7 N3 Al1 112.5(3) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 C4 109.5(2) . . ?
N1 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
N1 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
N2 C4 C3 108.9(2) . . ?
N2 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
N2 C4 H4B 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
N2 C5 C6 108.6(2) . . ?
N2 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
N2 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
N3 C6 C5 109.7(2) . . ?
N3 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
N3 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
N3 Ga1 N2 C5 29.9(5) . . . . ?
N1 Ga1 N2 C5 -142.1(3) . . . . ?
N3 Ga1 N2 C4 148.4(3) . . . . ?
N1 Ga1 N2 C4 -23.6(5) . . . . ?
N3 Ga1 N2 Ga2 -89.4(5) . . . . ?
N1 Ga1 N2 Ga2 98.7(4) . . . . ?
C1 N1 C3 C4 153.2(3) . . . . ?
C2 N1 C3 C4 -86.8(3) . . . . ?
Al1 N1 C3 C4 32.0(3) . . . . ?
Ga1 N1 C3 C4 31.4(4) . . . . ?
C5 N2 C4 C3 164.9(2) . . . . ?
Ga1 N2 C4 C3 49.2(6) . . . . ?
Al1 N2 C4 C3 48.2(4) . . . . ?
Ga2 N2 C4 C3 -76.2(3) . . . . ?
N1 C3 C4 N2 -53.9(3) . . . . ?
C4 N2 C5 C6 -171.4(2) . . . . ?
Ga1 N2 C5 C6 -52.6(6) . . . . ?
Al1 N2 C5 C6 -53.8(4) . . . . ?
Ga2 N2 C5 C6 69.9(3) . . . . ?
C8 N3 C6 C5 92.8(3) . . . . ?
C7 N3 C6 C5 -147.8(3) . . . . ?
Ga1 N3 C6 C5 -25.1(4) . . . . ?
Al1 N3 C6 C5 -24.8(3) . . . . ?
N2 C5 C6 N3 52.2(3) . . . . ?
 
_refine_diff_density_max    0.258
_refine_diff_density_min   -0.224
_refine_diff_density_rms    0.038

_shelxl_version_number 2014/6



