#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:02:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180056 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/02/7050212.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7050212
loop_
_publ_author_name
'Baker, Robert J.'
'Jones, Cameron'
'Kloth, Marc'
'Mills, David P.'
_publ_section_title
;
 The reactivity of gallium(i) and indium(i) halides towards
 bipyridines, terpyridines, imino-substituted pyridines and
 bis(imino)acenaphthenes
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              207
_journal_paper_doi               10.1039/b310592j
_journal_volume                  28
_journal_year                    2004
_chemical_formula_sum            'C33 H43 Ga2 I6 N3'
_chemical_formula_weight         1382.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.95(3)
_cell_angle_beta                 86.76(3)
_cell_angle_gamma                81.91(3)
_cell_formula_units_Z            2
_cell_length_a                   10.285(2)
_cell_length_b                   13.001(3)
_cell_length_c                   16.458(3)
_cell_measurement_temperature    150(2)
_cell_volume                     2121.8(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1385
_diffrn_reflns_av_sigmaI/netI    0.0960
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26217
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    5.660
_exptl_absorpt_correction_T_max  0.524
_exptl_absorpt_correction_T_min  0.241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.006
_refine_diff_density_min         -2.507
_refine_diff_density_rms         0.277
_refine_ls_extinction_coef       0.0052(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         7606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0655
_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/[σ²(Fo²)+(0.0829P)²+8.2456P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1757
_reflns_number_gt                6113
_reflns_number_total             7606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b310592j.txt
_cod_data_source_block           compound_8
_cod_original_cell_volume        2121.8(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050212
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
I1 I 0.93011(7) 0.70104(6) 0.27278(5) 0.0428(2) Uani 1 1 d . . .
I2 I 0.60562(7) 0.53151(5) 0.39054(4) 0.0397(2) Uani 1 1 d . . .
I3 I 1.24983(7) 0.88849(5) 0.15880(5) 0.0452(2) Uani 1 1 d . . .
I4 I 1.00510(8) 1.15609(6) 0.03287(5) 0.0521(3) Uani 1 1 d . . .
I5 I 1.27403(7) 1.17793(5) 0.20800(4) 0.0397(2) Uani 1 1 d . . .
I6 I 0.93726(7) 1.03913(7) 0.28651(5) 0.0511(3) Uani 1 1 d . . .
Ga1 Ga 0.68566(10) 0.68667(8) 0.29218(6) 0.0275(3) Uani 1 1 d . . .
Ga2 Ga 1.11192(11) 1.06470(8) 0.17036(7) 0.0345(3) Uani 1 1 d . . .
N1 N 0.6233(7) 0.8051(6) 0.3664(4) 0.0274(16) Uani 1 1 d . . .
N2 N 0.6337(7) 0.8219(6) 0.2067(5) 0.0280(16) Uani 1 1 d . . .
N3 N 0.6516(8) 0.6342(7) 0.1764(5) 0.0320(18) Uani 1 1 d . . .
C1 C 0.6104(10) 0.9028(8) 0.3250(6) 0.034(2) Uani 1 1 d . . .
C2 C 0.6468(10) 0.7098(7) 0.1113(6) 0.031(2) Uani 1 1 d . . .
C3 C 0.5771(10) 0.9995(8) 0.3571(7) 0.036(2) Uani 1 1 d . . .
H3A H 0.5533 0.9803 0.4166 0.054 Uiso 1 1 calc R . .
H3B H 0.5027 1.0442 0.3267 0.054 Uiso 1 1 calc R . .
H3C H 0.6530 1.0390 0.3496 0.054 Uiso 1 1 calc R . .
C4 C 0.6399(14) 0.6963(10) 0.0235(7) 0.055(3) Uani 1 1 d . . .
H4A H 0.7234 0.7090 -0.0062 0.083 Uiso 1 1 calc R . .
H4B H 0.5686 0.7473 -0.0051 0.083 Uiso 1 1 calc R . .
H4C H 0.6231 0.6236 0.0245 0.083 Uiso 1 1 calc R . .
C5 C 0.5906(10) 0.7825(7) 0.4537(6) 0.032(2) Uani 1 1 d . . .
C6 C 0.6900(11) 0.7491(8) 0.5125(6) 0.036(2) Uani 1 1 d . . .
C7 C 0.6486(11) 0.7228(9) 0.5954(6) 0.042(3) Uani 1 1 d . . .
H7 H 0.7139 0.7023 0.6366 0.051 Uiso 1 1 calc R . .
C8 C 0.5233(12) 0.7243(8) 0.6209(6) 0.042(3) Uani 1 1 d . . .
H8 H 0.5021 0.7032 0.6787 0.050 Uiso 1 1 calc R . .
C9 C 0.4211(12) 0.7572(8) 0.5624(7) 0.043(3) Uani 1 1 d . . .
H9 H 0.3315 0.7608 0.5803 0.052 Uiso 1 1 calc R . .
C10 C 0.4563(11) 0.7845(8) 0.4768(6) 0.038(2) Uani 1 1 d . . .
C11 C 0.8336(11) 0.7441(9) 0.4902(7) 0.046(3) Uani 1 1 d . . .
H11 H 0.8416 0.7660 0.4280 0.055 Uiso 1 1 calc R . .
C12 C 0.8996(13) 0.8241(12) 0.5265(8) 0.062(4) Uani 1 1 d . . .
H12A H 0.8484 0.8949 0.5119 0.093 Uiso 1 1 calc R . .
H12B H 0.9890 0.8274 0.5031 0.093 Uiso 1 1 calc R . .
H12C H 0.9029 0.8004 0.5873 0.093 Uiso 1 1 calc R . .
C13 C 0.9057(12) 0.6297(10) 0.5161(9) 0.061(4) Uani 1 1 d . . .
H13A H 0.9105 0.6091 0.5770 0.091 Uiso 1 1 calc R . .
H13B H 0.9948 0.6268 0.4914 0.091 Uiso 1 1 calc R . .
H13C H 0.8577 0.5805 0.4962 0.091 Uiso 1 1 calc R . .
C14 C 0.3475(10) 0.8202(9) 0.4159(7) 0.047(3) Uani 1 1 d . . .
H14 H 0.3877 0.8386 0.3586 0.056 Uiso 1 1 calc R . .
C15 C 0.2588(12) 0.9191(11) 0.4318(9) 0.064(4) Uani 1 1 d . . .
H15A H 0.2190 0.9029 0.4880 0.096 Uiso 1 1 calc R . .
H15B H 0.1895 0.9400 0.3906 0.096 Uiso 1 1 calc R . .
H15C H 0.3113 0.9776 0.4271 0.096 Uiso 1 1 calc R . .
C16 C 0.2611(12) 0.7318(12) 0.4183(8) 0.064(4) Uani 1 1 d . . .
H16A H 0.3149 0.6700 0.4035 0.097 Uiso 1 1 calc R . .
H16B H 0.1905 0.7583 0.3783 0.097 Uiso 1 1 calc R . .
H16C H 0.2229 0.7110 0.4745 0.097 Uiso 1 1 calc R . .
C17 C 0.6304(9) 0.5274(7) 0.1691(5) 0.029(2) Uani 1 1 d . . .
C18 C 0.5016(9) 0.5108(7) 0.1601(6) 0.029(2) Uani 1 1 d . . .
C19 C 0.4846(10) 0.4080(8) 0.1499(6) 0.036(2) Uani 1 1 d . . .
H19 H 0.3987 0.3931 0.1426 0.043 Uiso 1 1 calc R . .
C20 C 0.5887(11) 0.3297(8) 0.1502(7) 0.040(2) Uani 1 1 d . . .
H20 H 0.5749 0.2621 0.1420 0.048 Uiso 1 1 calc R . .
C21 C 0.7137(11) 0.3490(8) 0.1625(6) 0.043(3) Uani 1 1 d . . .
H21 H 0.7849 0.2936 0.1636 0.051 Uiso 1 1 calc R . .
C22 C 0.7379(9) 0.4467(8) 0.1732(6) 0.032(2) Uani 1 1 d . . .
C23 C 0.3812(10) 0.5913(8) 0.1631(7) 0.041(2) Uani 1 1 d . . .
H23 H 0.4103 0.6589 0.1702 0.049 Uiso 1 1 calc R . .
C24 C 0.3067(13) 0.6151(11) 0.0815(9) 0.062(3) Uani 1 1 d . . .
H24A H 0.3609 0.6506 0.0356 0.093 Uiso 1 1 calc R . .
H24B H 0.2244 0.6617 0.0867 0.093 Uiso 1 1 calc R . .
H24C H 0.2870 0.5483 0.0699 0.093 Uiso 1 1 calc R . .
C25 C 0.2904(11) 0.5517(10) 0.2371(7) 0.047(3) Uani 1 1 d . . .
H25A H 0.2495 0.4924 0.2266 0.071 Uiso 1 1 calc R . .
H25B H 0.2220 0.6099 0.2441 0.071 Uiso 1 1 calc R . .
H25C H 0.3417 0.5276 0.2879 0.071 Uiso 1 1 calc R . .
C26 C 0.8763(11) 0.4668(9) 0.1853(8) 0.050(3) Uani 1 1 d . . .
H26 H 0.8701 0.5395 0.1971 0.060 Uiso 1 1 calc R . .
C27 C 0.9574(14) 0.4679(14) 0.1059(10) 0.080(5) Uani 1 1 d . . .
H27A H 0.9700 0.3965 0.0941 0.121 Uiso 1 1 calc R . .
H27B H 1.0431 0.4895 0.1123 0.121 Uiso 1 1 calc R . .
H27C H 0.9118 0.5185 0.0596 0.121 Uiso 1 1 calc R . .
C28 C 0.9389(13) 0.3883(12) 0.2600(9) 0.070(4) Uani 1 1 d . . .
H28A H 0.8788 0.3861 0.3086 0.105 Uiso 1 1 calc R . .
H28B H 1.0213 0.4110 0.2720 0.105 Uiso 1 1 calc R . .
H28C H 0.9568 0.3173 0.2477 0.105 Uiso 1 1 calc R . .
C29 C 0.6250(10) 0.9139(7) 0.2312(6) 0.031(2) Uani 1 1 d . . .
C30 C 0.6363(10) 1.0104(8) 0.1719(6) 0.037(2) Uani 1 1 d . . .
H30 H 0.6365 1.0757 0.1887 0.044 Uiso 1 1 calc R . .
C31 C 0.6468(11) 1.0054(8) 0.0896(6) 0.040(2) Uani 1 1 d . . .
H31 H 0.6512 1.0692 0.0484 0.048 Uiso 1 1 calc R . .
C32 C 0.6512(10) 0.9091(8) 0.0641(6) 0.036(2) Uani 1 1 d . . .
H32 H 0.6577 0.9064 0.0069 0.044 Uiso 1 1 calc R . .
C33 C 0.6455(10) 0.8183(7) 0.1264(6) 0.034(2) Uani 1 1 d . . .
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'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N2 Ga1 N1 75.9(3) . . ?
N2 Ga1 N3 74.8(3) . . ?
N1 Ga1 N3 145.0(3) . . ?
N2 Ga1 I2 145.5(2) . . ?
N1 Ga1 I2 97.4(2) . . ?
N3 Ga1 I2 95.9(2) . . ?
N2 Ga1 I1 93.7(2) . . ?
N1 Ga1 I1 101.0(2) . . ?
N3 Ga1 I1 99.6(2) . . ?
I2 Ga1 I1 120.74(5) . . ?
I4 Ga2 I6 109.93(5) . . ?
I4 Ga2 I3 110.83(5) . . ?
I6 Ga2 I3 111.98(5) . . ?
I4 Ga2 I5 110.47(5) . . ?
I6 Ga2 I5 108.28(5) . . ?
I3 Ga2 I5 105.24(5) . . ?
C1 N1 C5 119.4(8) . . ?
C1 N1 Ga1 115.0(6) . . ?
C5 N1 Ga1 125.6(6) . . ?
C33 N2 C29 121.5(8) . . ?
C33 N2 Ga1 118.1(6) . . ?
C29 N2 Ga1 117.6(6) . . ?
C2 N3 C17 119.5(8) . . ?
C2 N3 Ga1 113.1(6) . . ?
C17 N3 Ga1 127.4(6) . . ?
N1 C1 C3 128.0(9) . . ?
N1 C1 C29 113.6(8) . . ?
C3 C1 C29 118.3(8) . . ?
N3 C2 C33 115.6(8) . . ?
N3 C2 C4 125.0(9) . . ?
C33 C2 C4 119.3(9) . . ?
C6 C5 C10 122.1(9) . . ?
C6 C5 N1 120.3(9) . . ?
C10 C5 N1 117.2(9) . . ?
C7 C6 C5 116.2(10) . . ?
C7 C6 C11 120.1(10) . . ?
C5 C6 C11 123.7(9) . . ?
C8 C7 C6 124.3(10) . . ?
C7 C8 C9 120.5(9) . . ?
C10 C9 C8 118.2(10) . . ?
C5 C10 C9 118.6(10) . . ?
C5 C10 C14 123.7(9) . . ?
C9 C10 C14 117.6(10) . . ?
C6 C11 C13 111.8(10) . . ?
C6 C11 C12 111.8(9) . . ?
C13 C11 C12 111.5(10) . . ?
C10 C14 C15 112.1(10) . . ?
C10 C14 C16 111.8(10) . . ?
C15 C14 C16 108.3(10) . . ?
C18 C17 C22 123.1(8) . . ?
C18 C17 N3 117.2(8) . . ?
C22 C17 N3 119.7(8) . . ?
C17 C18 C19 116.0(9) . . ?
C17 C18 C23 125.4(8) . . ?
C19 C18 C23 118.6(8) . . ?
C20 C19 C18 121.7(9) . . ?
C19 C20 C21 120.0(9) . . ?
C20 C21 C22 121.6(10) . . ?
C21 C22 C17 117.5(9) . . ?
C21 C22 C26 120.8(9) . . ?
C17 C22 C26 121.7(9) . . ?
C18 C23 C25 110.9(9) . . ?
C18 C23 C24 110.7(9) . . ?
C25 C23 C24 110.1(10) . . ?
C27 C26 C22 110.3(10) . . ?
C27 C26 C28 112.8(11) . . ?
C22 C26 C28 111.6(10) . . ?
N2 C29 C30 120.4(8) . . ?
N2 C29 C1 114.2(8) . . ?
C30 C29 C1 125.3(8) . . ?
C31 C30 C29 117.1(9) . . ?
C30 C31 C32 122.0(9) . . ?
C33 C32 C31 116.9(9) . . ?
N2 C33 C32 121.9(9) . . ?
N2 C33 C2 113.7(8) . . ?
C32 C33 C2 124.4(9) . . ?
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
I1 Ga1 2.5442(13) . ?
I2 Ga1 2.4919(14) . ?
I3 Ga2 2.5589(15) . ?
I4 Ga2 2.5374(15) . ?
I5 Ga2 2.5594(14) . ?
I6 Ga2 2.5466(16) . ?
Ga1 N2 2.014(7) . ?
Ga1 N1 2.182(7) . ?
Ga1 N3 2.225(8) . ?
N1 C1 1.291(12) . ?
N1 C5 1.429(12) . ?
N2 C33 1.331(12) . ?
N2 C29 1.336(12) . ?
N3 C2 1.278(12) . ?
N3 C17 1.467(12) . ?
C1 C3 1.463(13) . ?
C1 C29 1.518(13) . ?
C2 C33 1.485(13) . ?
C2 C4 1.500(13) . ?
C5 C6 1.402(14) . ?
C5 C10 1.410(15) . ?
C6 C7 1.387(14) . ?
C6 C11 1.497(16) . ?
C7 C8 1.331(16) . ?
C8 C9 1.421(16) . ?
C9 C10 1.412(14) . ?
C10 C14 1.497(15) . ?
C11 C13 1.544(16) . ?
C11 C12 1.558(15) . ?
C14 C15 1.533(18) . ?
C14 C16 1.541(18) . ?
C17 C18 1.393(13) . ?
C17 C22 1.406(13) . ?
C18 C19 1.421(13) . ?
C18 C23 1.511(14) . ?
C19 C20 1.369(14) . ?
C20 C21 1.378(16) . ?
C21 C22 1.380(14) . ?
C22 C26 1.514(14) . ?
C23 C25 1.531(15) . ?
C23 C24 1.533(16) . ?
C26 C27 1.508(19) . ?
C26 C28 1.518(18) . ?
C29 C30 1.419(13) . ?
C30 C31 1.370(14) . ?
C31 C32 1.400(14) . ?
C32 C33 1.384(13) . ?
