# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013


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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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data_rw03_0m
_database_code_depnum_ccdc_archive 'CCDC 905132'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '2(C4 H12 N), C3 H9 Cl6 Ga2 N Sn'
_chemical_formula_sum            'C11 H33 Cl6 Ga2 N3 Sn'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_exptl_crystal_recrystallization_method acetonitrile/tetrahydrofuran
_chemical_melting_point          ?
_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         678.23
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'
Cl Cl 0.1484 0.1585 '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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_int_tables_number      19
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_as_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                   11.5910(4)
_cell_length_b                   14.2637(5)
_cell_length_c                   15.6726(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2591.16(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9938
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      29.50
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    3.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3494
_exptl_absorpt_correction_T_max  0.4640
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_special_details           
;
?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56221
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         31.00
_reflns_number_total             8070
_reflns_number_gt                7049
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.8381P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(8)
_refine_ls_number_reflns         8070
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0551
_refine_ls_wR_factor_gt          0.0523
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.099687(14) 0.340583(11) 0.955341(12) 0.02994(4) Uani 1 1 d . . .
Ga1 Ga -0.11002(2) 0.49714(2) 0.946941(19) 0.03113(6) Uani 1 1 d . . .
Ga2 Ga 0.13822(2) 0.556537(18) 0.887960(18) 0.02646(6) Uani 1 1 d . . .
Cl1 Cl -0.15567(7) 0.64395(6) 0.91944(5) 0.04930(19) Uani 1 1 d . . .
Cl2 Cl -0.25656(7) 0.41275(7) 0.89854(6) 0.0614(3) Uani 1 1 d . . .
Cl3 Cl -0.12552(7) 0.48274(5) 1.08865(5) 0.04463(17) Uani 1 1 d . . .
Cl4 Cl 0.10498(7) 0.65223(5) 0.77974(5) 0.04648(16) Uani 1 1 d . . .
Cl5 Cl 0.17470(6) 0.64910(5) 0.99843(4) 0.03855(15) Uani 1 1 d . . .
Cl6 Cl 0.31326(6) 0.49961(5) 0.85750(5) 0.04602(18) Uani 1 1 d . . .
N1 N 0.03240(17) 0.46217(14) 0.90482(14) 0.0281(4) Uani 1 1 d . . .
C1 C 0.1818(3) 0.2643(2) 0.8551(2) 0.0430(7) Uani 1 1 d . . .
H1A H 0.2459 0.3013 0.8321 0.064 Uiso 1 1 calc R . .
H1B H 0.1259 0.2517 0.8096 0.064 Uiso 1 1 calc R . .
H1C H 0.2114 0.2048 0.8775 0.064 Uiso 1 1 calc R . .
C2 C -0.0372(3) 0.2540(2) 1.0010(2) 0.0486(8) Uani 1 1 d . . .
H2A H -0.0868 0.2357 0.9532 0.073 Uiso 1 1 calc R . .
H2B H -0.0828 0.2887 1.0431 0.073 Uiso 1 1 calc R . .
H2C H -0.0049 0.1977 1.0277 0.073 Uiso 1 1 calc R . .
C3 C 0.2117(3) 0.3829(2) 1.0566(2) 0.0432(7) Uani 1 1 d . . .
H3A H 0.2736 0.4223 1.0336 0.065 Uiso 1 1 calc R . .
H3B H 0.2453 0.3273 1.0836 0.065 Uiso 1 1 calc R . .
H3C H 0.1677 0.4186 1.0990 0.065 Uiso 1 1 calc R . .
N2 N 0.98386(19) 0.74916(16) 0.20315(14) 0.0321(5) Uani 1 1 d . . .
C4 C 1.0312(4) 0.6572(3) 0.2278(3) 0.0653(11) Uani 1 1 d . . .
H4A H 0.9677 0.6144 0.2415 0.098 Uiso 1 1 calc R . .
H4B H 1.0809 0.6646 0.2779 0.098 Uiso 1 1 calc R . .
H4C H 1.0763 0.6315 0.1804 0.098 Uiso 1 1 calc R . .
C5 C 0.9101(3) 0.7383(2) 0.1267(2) 0.0507(8) Uani 1 1 d . . .
H5A H 0.8472 0.6946 0.1392 0.076 Uiso 1 1 calc R . .
H5B H 0.9564 0.7139 0.0793 0.076 Uiso 1 1 calc R . .
H5C H 0.8778 0.7994 0.1108 0.076 Uiso 1 1 calc R . .
C6 C 1.0785(3) 0.8148(3) 0.1838(3) 0.0635(10) Uani 1 1 d . . .
H6A H 1.0463 0.8762 0.1690 0.095 Uiso 1 1 calc R . .
H6B H 1.1237 0.7908 0.1357 0.095 Uiso 1 1 calc R . .
H6C H 1.1285 0.8211 0.2339 0.095 Uiso 1 1 calc R . .
C7 C 0.9132(4) 0.7884(3) 0.2739(2) 0.0696(12) Uani 1 1 d . . .
H7A H 0.8509 0.7446 0.2879 0.104 Uiso 1 1 calc R . .
H7B H 0.8801 0.8486 0.2561 0.104 Uiso 1 1 calc R . .
H7C H 0.9621 0.7980 0.3241 0.104 Uiso 1 1 calc R . .
N3 N 0.5283(2) 0.56581(16) 0.12790(14) 0.0321(5) Uani 1 1 d . . .
C8 C 0.6040(3) 0.5631(4) 0.2032(2) 0.0710(11) Uani 1 1 d . . .
H8A H 0.6821 0.5452 0.1856 0.106 Uiso 1 1 calc R . .
H8B H 0.5743 0.5171 0.2441 0.106 Uiso 1 1 calc R . .
H8C H 0.6060 0.6252 0.2299 0.106 Uiso 1 1 calc R . .
C9 C 0.5752(4) 0.6359(3) 0.0668(3) 0.0723(12) Uani 1 1 d . . .
H9A H 0.5271 0.6371 0.0154 0.108 Uiso 1 1 calc R . .
H9B H 0.6544 0.6186 0.0513 0.108 Uiso 1 1 calc R . .
H9C H 0.5752 0.6980 0.0934 0.108 Uiso 1 1 calc R . .
C10 C 0.4097(3) 0.5916(3) 0.1554(3) 0.0626(10) Uani 1 1 d . . .
H10A H 0.3582 0.5915 0.1058 0.094 Uiso 1 1 calc R . .
H10B H 0.4107 0.6542 0.1811 0.094 Uiso 1 1 calc R . .
H10C H 0.3820 0.5459 0.1974 0.094 Uiso 1 1 calc R . .
C11 C 0.5265(4) 0.4731(2) 0.0864(3) 0.0654(11) Uani 1 1 d . . .
H11A H 0.4759 0.4752 0.0364 0.098 Uiso 1 1 calc R . .
H11B H 0.4977 0.4261 0.1268 0.098 Uiso 1 1 calc R . .
H11C H 0.6049 0.4563 0.0685 0.098 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sn1 0.02445(8) 0.02393(7) 0.04142(9) -0.00236(7) 0.00512(8) -0.00194(6)
Ga1 0.01955(12) 0.03496(14) 0.03887(15) -0.00996(12) 0.00222(11) 0.00123(11)
Ga2 0.02324(13) 0.02239(12) 0.03375(14) -0.00426(11) 0.00210(11) -0.00163(10)
Cl1 0.0420(4) 0.0462(4) 0.0597(4) -0.0016(3) -0.0025(3) 0.0185(3)
Cl2 0.0286(4) 0.0846(7) 0.0711(6) -0.0279(5) 0.0012(4) -0.0179(4)
Cl3 0.0464(4) 0.0464(4) 0.0410(4) -0.0071(3) 0.0104(3) 0.0012(3)
Cl4 0.0563(4) 0.0416(4) 0.0416(4) 0.0081(3) -0.0050(4) -0.0045(4)
Cl5 0.0393(4) 0.0344(3) 0.0419(4) -0.0122(3) -0.0059(3) -0.0016(3)
Cl6 0.0306(3) 0.0316(3) 0.0759(5) -0.0021(3) 0.0215(3) 0.0005(3)
N1 0.0199(10) 0.0243(10) 0.0402(12) -0.0059(9) 0.0028(9) -0.0021(7)
C1 0.0399(16) 0.0321(14) 0.0570(19) -0.0061(13) 0.0089(14) 0.0079(12)
C2 0.0418(17) 0.0352(15) 0.069(2) -0.0020(15) 0.0142(16) -0.0130(13)
C3 0.0350(15) 0.0467(17) 0.0479(18) 0.0048(14) -0.0058(13) -0.0020(12)
N2 0.0306(11) 0.0365(12) 0.0292(11) 0.0006(10) -0.0026(9) 0.0041(9)
C4 0.075(3) 0.052(2) 0.069(2) 0.004(2) -0.025(2) 0.020(2)
C5 0.055(2) 0.0511(18) 0.0462(17) -0.0055(14) -0.0153(16) 0.0093(16)
C6 0.050(2) 0.071(2) 0.069(2) 0.0098(19) -0.0076(18) -0.0182(18)
C7 0.075(3) 0.087(3) 0.047(2) 0.0030(19) 0.016(2) 0.023(2)
N3 0.0324(12) 0.0303(11) 0.0337(12) -0.0002(9) 0.0027(9) -0.0004(9)
C8 0.047(2) 0.117(3) 0.0489(19) 0.004(2) -0.0004(17) -0.009(2)
C9 0.090(3) 0.056(2) 0.071(3) 0.0205(19) 0.014(2) -0.019(2)
C10 0.0387(19) 0.070(2) 0.079(2) -0.005(2) 0.0064(18) 0.0140(17)
C11 0.061(2) 0.0400(18) 0.096(3) -0.0176(18) 0.016(2) -0.0122(16)
_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
Sn1 N1 2.060(2) . ?
Sn1 C2 2.135(3) . ?
Sn1 C1 2.136(3) . ?
Sn1 C3 2.138(3) . ?
Ga1 N1 1.847(2) . ?
Ga1 Cl1 2.2024(8) . ?
Ga1 Cl2 2.2158(8) . ?
Ga1 Cl3 2.2376(8) . ?
Ga2 N1 1.840(2) . ?
Ga2 Cl4 2.2110(8) . ?
Ga2 Cl5 2.2180(7) . ?
Ga2 Cl6 2.2368(7) . ?
N2 C4 1.473(4) . ?
N2 C6 1.474(4) . ?
N2 C5 1.481(4) . ?
N2 C7 1.488(4) . ?
N3 C8 1.471(4) . ?
N3 C11 1.474(4) . ?
N3 C10 1.487(4) . ?
N3 C9 1.487(4) . ?
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
N1 Sn1 C2 109.55(11) . . ?
N1 Sn1 C1 108.37(10) . . ?
C2 Sn1 C1 106.44(13) . . ?
N1 Sn1 C3 106.11(10) . . ?
C2 Sn1 C3 111.49(14) . . ?
C1 Sn1 C3 114.79(13) . . ?
N1 Ga1 Cl1 113.68(7) . . ?
N1 Ga1 Cl2 114.59(7) . . ?
Cl1 Ga1 Cl2 105.39(4) . . ?
N1 Ga1 Cl3 113.69(8) . . ?
Cl1 Ga1 Cl3 105.20(3) . . ?
Cl2 Ga1 Cl3 103.20(4) . . ?
N1 Ga2 Cl4 116.46(7) . . ?
N1 Ga2 Cl5 116.77(7) . . ?
Cl4 Ga2 Cl5 105.34(3) . . ?
N1 Ga2 Cl6 111.70(7) . . ?
Cl4 Ga2 Cl6 102.62(3) . . ?
Cl5 Ga2 Cl6 102.11(3) . . ?
Ga2 N1 Ga1 116.72(11) . . ?
Ga2 N1 Sn1 114.75(10) . . ?
Ga1 N1 Sn1 115.38(11) . . ?
C4 N2 C6 110.0(3) . . ?
C4 N2 C5 109.6(3) . . ?
C6 N2 C5 109.3(3) . . ?
C4 N2 C7 110.2(3) . . ?
C6 N2 C7 108.9(3) . . ?
C5 N2 C7 108.9(3) . . ?
C8 N3 C11 109.8(3) . . ?
C8 N3 C10 109.0(3) . . ?
C11 N3 C10 109.7(3) . . ?
C8 N3 C9 108.4(3) . . ?
C11 N3 C9 108.9(3) . . ?
C10 N3 C9 111.0(3) . . ?
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        31.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.082


data_rw45b_0m
_database_code_depnum_ccdc_archive 'CCDC 905133'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '3(C4 H12 N), Cl9 Ga3 N'
_chemical_formula_sum            'C12 H36 Cl9 Ga3 N4'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_exptl_crystal_recrystallization_method acetontrile/THF
_chemical_melting_point          ?
_exptl_crystal_description       'triangular plate'
_exptl_crystal_colour            colorless
_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         764.66
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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_H-M   'R 3'
_symmetry_int_tables_number      146
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
_cell_length_a                   10.7081(18)
_cell_length_b                   10.7081(18)
_cell_length_c                   22.379(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2222.3(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3500
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      24.82
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1146
_exptl_absorpt_coefficient_mu    3.529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6590
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_special_details           
;
?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12536
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         30.48
_reflns_number_total             2856
_reflns_number_gt                2327
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+1.0855P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(12)
_refine_ls_number_reflns         2856
_refine_ls_number_parameters     141
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0689
_refine_ls_wR_factor_gt          0.0644
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.06792(5) 0.19408(5) 0.00857(2) 0.02422(12) Uani 0.50 1 d P A 1
Cl1 Cl 0.3058(3) 0.3257(3) 0.00177(14) 0.0442(6) Uani 0.50 1 d P A 1
Cl2 Cl 0.0090(2) 0.3037(2) 0.08138(11) 0.0367(4) Uani 0.50 1 d P A 1
Cl3 Cl -0.0103(3) 0.2418(3) -0.07222(11) 0.0473(5) Uani 0.50 1 d P A 1
N1 N 0.0000 0.0000 0.0271(4) 0.0215(16) Uani 0.50 3 d SP . 1
Ga2 Ga 0.19406(5) 0.06787(5) 0.01314(2) 0.02430(12) Uani 0.50 1 d P . 2
Cl4 Cl 0.3258(3) 0.3058(3) 0.01991(14) 0.0443(6) Uani 0.50 1 d P B 2
Cl5 Cl -0.0090(2) 0.2948(2) -0.05970(11) 0.0367(4) Uani 0.50 1 d P C 2
Cl6 Cl 0.0106(3) 0.2521(3) 0.09392(11) 0.0474(5) Uani 0.50 1 d P D 2
N2 N 0.0000 0.0000 -0.0049(5) 0.0223(16) Uani 0.50 3 d SP . 2
N3 N 0.6667 0.3333 0.8343(7) 0.049(3) Uani 0.497(13) 3 d SPD . 1
C1 C 0.796(5) 0.466(5) 0.854(3) 0.116(10) Uani 0.497(13) 1 d PD . 1
H1A H 0.7949 0.5501 0.8373 0.175 Uiso 0.497(13) 1 calc PR . 1
H1B H 0.8824 0.4653 0.8409 0.175 Uiso 0.497(13) 1 calc PR . 1
H1C H 0.7958 0.4716 0.8980 0.175 Uiso 0.497(13) 1 calc PR . 1
C2 C 0.6667 0.3333 0.7679(6) 0.095(4) Uani 0.497(13) 3 d SPD . 1
H2A H 0.6735 0.4228 0.7534 0.142 Uiso 0.166(4) 1 calc PR . 1
H2B H 0.5772 0.2507 0.7534 0.142 Uiso 0.166(4) 1 calc PR . 1
H2C H 0.7493 0.3265 0.7534 0.142 Uiso 0.166(4) 1 calc PR . 1
N4 N 0.6667 0.3333 0.8535(7) 0.049(3) Uani 0.503(13) 3 d SPD . 2
C3 C 0.800(5) 0.463(5) 0.834(3) 0.116(10) Uani 0.503(13) 1 d PD . 2
H3A H 0.8038 0.4656 0.7899 0.175 Uiso 0.503(13) 1 calc PR . 2
H3B H 0.8839 0.4591 0.8492 0.175 Uiso 0.503(13) 1 calc PR . 2
H3C H 0.8016 0.5492 0.8488 0.175 Uiso 0.503(13) 1 calc PR . 2
C4 C 0.6667 0.3333 0.9197(6) 0.095(4) Uani 0.503(13) 3 d SPD . 2
H4A H 0.6602 0.4162 0.9343 0.142 Uiso 0.168(4) 1 calc PR . 2
H4B H 0.7560 0.3398 0.9343 0.142 Uiso 0.168(4) 1 calc PR . 2
H4C H 0.5838 0.2440 0.9343 0.142 Uiso 0.168(4) 1 calc PR . 2
N5 N 0.0000 0.0000 0.2202(4) 0.0425(18) Uani 0.618(4) 3 d SPD . 1
C5 C 0.1266(7) 0.1370(7) 0.1979(3) 0.0515(14) Uani 0.618(4) 1 d PD . 1
H5A H 0.2161 0.1436 0.2124 0.077 Uiso 0.618(4) 1 calc PR . 1
H5B H 0.1199 0.2197 0.2125 0.077 Uiso 0.618(4) 1 calc PR . 1
H5C H 0.1264 0.1370 0.1541 0.077 Uiso 0.618(4) 1 calc PR . 1
C6 C 0.0000 0.0000 0.2875(5) 0.050(2) Uani 0.618(4) 3 d SPD . 1
H6A H 0.0901 0.0081 0.3021 0.075 Uiso 0.2059(14) 1 calc PR . 1
H6B H -0.0819 -0.0901 0.3021 0.075 Uiso 0.2059(14) 1 calc PR . 1
H6C H -0.0081 0.0819 0.3021 0.075 Uiso 0.2059(14) 1 calc PR . 1
N6 N 0.0000 0.0000 0.2531(7) 0.0425(18) Uani 0.382(4) 3 d SPD . 2
C7 C 0.1179(12) 0.1421(11) 0.2304(5) 0.0515(14) Uani 0.382(4) 1 d PD . 2
H7A H 0.1175 0.1416 0.1866 0.077 Uiso 0.382(4) 1 calc PR . 2
H7B H 0.2111 0.1582 0.2449 0.077 Uiso 0.382(4) 1 calc PR . 2
H7C H 0.1021 0.2195 0.2449 0.077 Uiso 0.382(4) 1 calc PR . 2
C8 C 0.0000 0.0000 0.3193(8) 0.050(2) Uani 0.382(4) 3 d SPD . 2
H8A H 0.0949 0.0213 0.3339 0.075 Uiso 0.1274(14) 1 calc PR . 2
H8B H -0.0737 -0.0949 0.3339 0.075 Uiso 0.1274(14) 1 calc PR . 2
H8C H -0.0213 0.0737 0.3339 0.075 Uiso 0.1274(14) 1 calc PR . 2
N7 N 0.0000 0.0000 0.8018(4) 0.0416(18) Uani 0.618(4) 3 d SPD . 1
C9 C 0.0000 0.0000 0.7345(5) 0.054(2) Uani 0.618(4) 3 d SPD . 1
H9A H -0.0900 -0.0821 0.7199 0.080 Uiso 0.2059(14) 1 calc PR . 1
H9B H 0.0821 -0.0079 0.7199 0.080 Uiso 0.2059(14) 1 calc PR . 1
H9C H 0.0079 0.0900 0.7199 0.080 Uiso 0.2059(14) 1 calc PR . 1
C10 C 0.1362(6) 0.1265(7) 0.8243(3) 0.0513(14) Uani 0.618(4) 1 d PD . 1
H10A H 0.1429 0.2159 0.8095 0.077 Uiso 0.618(4) 1 calc PR . 1
H10B H 0.2192 0.1199 0.8100 0.077 Uiso 0.618(4) 1 calc PR . 1
H10C H 0.1355 0.1266 0.8680 0.077 Uiso 0.618(4) 1 calc PR . 1
N8 N 0.0000 0.0000 0.7684(7) 0.0416(18) Uani 0.382(4) 3 d SPD . 2
C11 C 0.0000 0.0000 0.7024(8) 0.054(2) Uani 0.382(4) 3 d SPD . 2
H11A H -0.0940 -0.0757 0.6878 0.080 Uiso 0.1274(14) 1 calc PR . 2
H11B H 0.0757 -0.0183 0.6878 0.080 Uiso 0.1274(14) 1 calc PR . 2
H11C H 0.0183 0.0940 0.6878 0.080 Uiso 0.1274(14) 1 calc PR . 2
C12 C 0.1423(10) 0.1171(11) 0.7907(6) 0.0513(14) Uani 0.382(4) 1 d PD . 2
H12A H 0.1422 0.1170 0.8345 0.077 Uiso 0.382(4) 1 calc PR . 2
H12B H 0.1588 0.2105 0.7762 0.077 Uiso 0.382(4) 1 calc PR . 2
H12C H 0.2192 0.1006 0.7761 0.077 Uiso 0.382(4) 1 calc PR . 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga1 0.0202(2) 0.0160(2) 0.0359(3) -0.0007(2) -0.0028(2) 0.0087(2)
Cl1 0.0222(9) 0.0248(10) 0.0768(18) 0.0095(10) -0.0068(10) 0.0051(7)
Cl2 0.0342(8) 0.0308(10) 0.0494(11) -0.0140(8) -0.0061(7) 0.0195(8)
Cl3 0.0550(11) 0.0464(14) 0.0379(11) 0.0122(10) -0.0055(8) 0.0233(12)
N1 0.018(3) 0.018(3) 0.028(4) 0.000 0.000 0.0092(13)
Ga2 0.0160(2) 0.0201(2) 0.0364(3) 0.0028(2) 0.0007(2) 0.0087(2)
Cl4 0.0255(10) 0.0213(9) 0.0770(18) 0.0071(10) -0.0097(10) 0.0048(7)
Cl5 0.0344(8) 0.0264(9) 0.0490(11) 0.0087(8) -0.0049(7) 0.0150(8)
Cl6 0.0549(11) 0.0555(15) 0.0378(11) -0.0186(10) -0.0068(8) 0.0320(12)
N2 0.018(3) 0.018(3) 0.031(4) 0.000 0.000 0.0089(13)
N3 0.0473(18) 0.0473(18) 0.053(9) 0.000 0.000 0.0237(9)
C1 0.058(3) 0.054(3) 0.21(3) -0.034(13) 0.034(13) 0.004(3)
C2 0.105(6) 0.105(6) 0.074(7) 0.000 0.000 0.053(3)
N4 0.0473(18) 0.0473(18) 0.053(9) 0.000 0.000 0.0237(9)
C3 0.058(3) 0.054(3) 0.21(3) -0.034(13) 0.034(13) 0.004(3)
C4 0.105(6) 0.105(6) 0.074(7) 0.000 0.000 0.053(3)
N5 0.0418(19) 0.0418(19) 0.044(5) 0.000 0.000 0.0209(10)
C5 0.047(2) 0.044(2) 0.059(4) 0.003(3) -0.002(4) 0.0193(19)
C6 0.058(3) 0.058(3) 0.034(6) 0.000 0.000 0.0291(14)
N6 0.0418(19) 0.0418(19) 0.044(5) 0.000 0.000 0.0209(10)
C7 0.047(2) 0.044(2) 0.059(4) 0.003(3) -0.002(4) 0.0193(19)
C8 0.058(3) 0.058(3) 0.034(6) 0.000 0.000 0.0291(14)
N7 0.0400(19) 0.0400(19) 0.045(5) 0.000 0.000 0.0200(9)
C9 0.065(3) 0.065(3) 0.031(5) 0.000 0.000 0.0326(16)
C10 0.041(2) 0.043(2) 0.064(4) -0.004(4) -0.003(3) 0.0170(18)
N8 0.0400(19) 0.0400(19) 0.045(5) 0.000 0.000 0.0200(9)
C11 0.065(3) 0.065(3) 0.031(5) 0.000 0.000 0.0326(16)
C12 0.041(2) 0.043(2) 0.064(4) -0.004(4) -0.003(3) 0.0170(18)
_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
Ga1 N1 1.873(2) . ?
Ga1 Cl3 2.159(2) . ?
Ga1 Cl1 2.215(3) . ?
Ga1 Cl2 2.275(2) . ?
N1 Ga1 1.873(2) 2 ?
N1 Ga1 1.873(2) 3 ?
Ga2 N2 1.871(2) . ?
Ga2 Cl6 2.159(2) 3 ?
Ga2 Cl4 2.216(3) . ?
Ga2 Cl5 2.275(2) 3 ?
Cl5 Ga2 2.275(2) 2 ?
Cl6 Ga2 2.159(2) 2 ?
N2 Ga2 1.871(2) 3 ?
N2 Ga2 1.871(2) 2 ?
N3 C1 1.473(17) 3_665 ?
N3 C1 1.473(18) . ?
N3 C1 1.473(17) 2_655 ?
N3 C2 1.485(17) . ?
N4 C3 1.476(17) 3_665 ?
N4 C3 1.476(18) . ?
N4 C3 1.476(17) 2_655 ?
N4 C4 1.483(17) . ?
N5 C5 1.500(6) 2 ?
N5 C5 1.500(6) . ?
N5 C5 1.500(6) 3 ?
N5 C6 1.505(10) . ?
N6 C8 1.483(13) . ?
N6 C7 1.498(9) 2 ?
N6 C7 1.498(10) . ?
N6 C7 1.498(9) 3 ?
N7 C10 1.496(6) . ?
N7 C10 1.496(6) 3 ?
N7 C10 1.496(6) 2 ?
N7 C9 1.505(10) . ?
N8 C11 1.477(13) . ?
N8 C12 1.494(9) . ?
N8 C12 1.494(9) 3 ?
N8 C12 1.494(9) 2 ?
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
N1 Ga1 Cl3 117.8(3) . . ?
N1 Ga1 Cl1 113.97(7) . . ?
Cl3 Ga1 Cl1 104.52(10) . . ?
N1 Ga1 Cl2 111.1(3) . . ?
Cl3 Ga1 Cl2 103.72(9) . . ?
Cl1 Ga1 Cl2 104.38(11) . . ?
Ga1 N1 Ga1 115.2(2) 2 . ?
Ga1 N1 Ga1 115.2(2) 2 3 ?
Ga1 N1 Ga1 115.2(2) . 3 ?
N2 Ga2 Cl6 117.5(3) . 3 ?
N2 Ga2 Cl4 113.98(7) . . ?
Cl6 Ga2 Cl4 104.58(10) 3 . ?
N2 Ga2 Cl5 111.4(3) . 3 ?
Cl6 Ga2 Cl5 103.74(9) 3 3 ?
Cl4 Ga2 Cl5 104.32(11) . 3 ?
Ga2 N2 Ga2 115.5(2) . 3 ?
Ga2 N2 Ga2 115.5(2) . 2 ?
Ga2 N2 Ga2 115.5(2) 3 2 ?
C1 N3 C1 111.2(19) 3_665 . ?
C1 N3 C1 111.2(19) 3_665 2_655 ?
C1 N3 C1 111.2(19) . 2_655 ?
C1 N3 C2 108(2) 3_665 . ?
C1 N3 C2 108(2) . . ?
C1 N3 C2 108(2) 2_655 . ?
C3 N4 C3 111.4(19) 3_665 . ?
C3 N4 C3 111.4(19) 3_665 2_655 ?
C3 N4 C3 111.4(18) . 2_655 ?
C3 N4 C4 107(2) 3_665 . ?
C3 N4 C4 107(2) . . ?
C3 N4 C4 107(2) 2_655 . ?
C5 N5 C5 109.5(4) 2 . ?
C5 N5 C5 109.5(4) 2 3 ?
C5 N5 C5 109.5(4) . 3 ?
C5 N5 C6 109.5(4) 2 . ?
C5 N5 C6 109.5(4) . . ?
C5 N5 C6 109.5(4) 3 . ?
C8 N6 C7 109.8(7) . 2 ?
C8 N6 C7 109.8(7) . . ?
C7 N6 C7 109.2(7) 2 . ?
C8 N6 C7 109.8(7) . 3 ?
C7 N6 C7 109.2(7) 2 3 ?
C7 N6 C7 109.2(7) . 3 ?
C10 N7 C10 109.3(4) . 3 ?
C10 N7 C10 109.3(4) . 2 ?
C10 N7 C10 109.3(4) 3 2 ?
C10 N7 C9 109.7(4) . . ?
C10 N7 C9 109.7(4) 3 . ?
C10 N7 C9 109.7(4) 2 . ?
C11 N8 C12 109.6(7) . . ?
C11 N8 C12 109.6(7) . 3 ?
C12 N8 C12 109.4(7) . 3 ?
C11 N8 C12 109.6(7) . 2 ?
C12 N8 C12 109.4(7) . 2 ?
C12 N8 C12 109.4(7) 3 2 ?
_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        30.48
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.058