#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:02:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180056 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/02/7050208.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_7050208
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            'C23 H18 Ga I3 N4'
_chemical_formula_weight         800.83
_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                99.44(3)
_cell_angle_beta                 97.59(3)
_cell_angle_gamma                102.53(3)
_cell_formula_units_Z            2
_cell_length_a                   7.3570(15)
_cell_length_b                   13.306(3)
_cell_length_c                   13.759(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1277.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0980
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22859
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    4.720
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.901
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0353P)²+1.3780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                3543
_reflns_number_total             4945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b310592j.txt
_cod_data_source_block           compound_4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050208
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 0.30048(7) 0.51971(4) 0.29720(3) 0.03498(15) Uani 1 1 d . . .
I2 I 0.78557(7) 0.40924(4) 0.40348(3) 0.03701(16) Uani 1 1 d . . .
I3 I 0.12907(7) 0.19330(4) -0.22844(3) 0.03275(15) Uani 1 1 d . . .
Ga1 Ga 0.47907(10) 0.37615(6) 0.28431(5) 0.02248(19) Uani 1 1 d . . .
N1 N 0.3141(8) 0.2784(4) 0.3603(4) 0.0234(13) Uani 1 1 d . . .
N2 N 0.3855(7) 0.2416(4) 0.1826(4) 0.0206(12) Uani 1 1 d . . .
N3 N 0.5966(7) 0.4143(4) 0.1585(4) 0.0234(13) Uani 1 1 d . . .
N4 N 0.5607(15) 0.0345(8) 0.3667(8) 0.086(3) Uani 1 1 d . . .
C1 C 0.2780(10) 0.3091(6) 0.4533(5) 0.0296(17) Uani 1 1 d . . .
H1 H 0.3300 0.3797 0.4876 0.036 Uiso 1 1 calc R . .
C2 C 0.1684(11) 0.2407(6) 0.4988(5) 0.0379(19) Uani 1 1 d . . .
H2 H 0.1442 0.2639 0.5638 0.045 Uiso 1 1 calc R . .
C3 C 0.0928(11) 0.1373(6) 0.4497(5) 0.0342(18) Uani 1 1 d . . .
H3 H 0.0159 0.0893 0.4805 0.041 Uiso 1 1 calc R . .
C4 C 0.1309(10) 0.1046(6) 0.3545(5) 0.0287(16) Uani 1 1 d . . .
H4 H 0.0823 0.0339 0.3198 0.034 Uiso 1 1 calc R . .
C5 C 0.2401(9) 0.1768(5) 0.3120(4) 0.0206(15) Uani 1 1 d . . .
C6 C 0.2862(9) 0.1564(5) 0.2094(4) 0.0185(14) Uani 1 1 d . . .
C7 C 0.2307(9) 0.0605(5) 0.1435(5) 0.0222(15) Uani 1 1 d . . .
H7 H 0.1636 0.0002 0.1636 0.027 Uiso 1 1 calc R . .
C8 C 0.2745(9) 0.0527(5) 0.0461(4) 0.0189(14) Uani 1 1 d . . .
C9 C 0.3728(9) 0.1444(5) 0.0210(5) 0.0225(15) Uani 1 1 d . . .
H9 H 0.4011 0.1425 -0.0445 0.027 Uiso 1 1 calc R . .
C10 C 0.4290(9) 0.2373(5) 0.0900(4) 0.0204(15) Uani 1 1 d . . .
C11 C 0.5425(9) 0.3366(5) 0.0739(5) 0.0207(15) Uani 1 1 d . . .
C12 C 0.5975(9) 0.3535(5) -0.0150(5) 0.0268(16) Uani 1 1 d . . .
H12 H 0.5542 0.3010 -0.0743 0.032 Uiso 1 1 calc R . .
C13 C 0.7182(10) 0.4495(6) -0.0156(5) 0.0310(17) Uani 1 1 d . . .
H13 H 0.7620 0.4624 -0.0754 0.037 Uiso 1 1 calc R . .
C14 C 0.7738(10) 0.5252(6) 0.0693(5) 0.0304(17) Uani 1 1 d . . .
H14 H 0.8553 0.5910 0.0686 0.036 Uiso 1 1 calc R . .
C15 C 0.7114(10) 0.5059(5) 0.1563(5) 0.0274(16) Uani 1 1 d . . .
H15 H 0.7510 0.5587 0.2155 0.033 Uiso 1 1 calc R . .
C16 C 0.2176(9) -0.0482(5) -0.0268(5) 0.0222(15) Uani 1 1 d . . .
C17 C 0.1228(9) -0.1410(5) -0.0008(5) 0.0252(16) Uani 1 1 d . . .
H17 H 0.0971 -0.1393 0.0653 0.030 Uiso 1 1 calc R . .
C18 C 0.0665(10) -0.2345(5) -0.0696(5) 0.0269(16) Uani 1 1 d . . .
H18 H -0.0009 -0.2957 -0.0510 0.032 Uiso 1 1 calc R . .
C19 C 0.1068(10) -0.2401(6) -0.1655(5) 0.0297(17) Uani 1 1 d . . .
H19 H 0.0685 -0.3047 -0.2128 0.036 Uiso 1 1 calc R . .
C20 C 0.2040(10) -0.1502(5) -0.1911(5) 0.0266(16) Uani 1 1 d . . .
H20 H 0.2342 -0.1535 -0.2564 0.032 Uiso 1 1 calc R . .
C21 C 0.2584(9) -0.0549(5) -0.1238(5) 0.0239(15) Uani 1 1 d . . .
H21 H 0.3237 0.0061 -0.1437 0.029 Uiso 1 1 calc R . .
C22 C 0.4164(14) -0.1605(8) 0.3722(8) 0.071(3) Uani 1 1 d . . .
H22A H 0.4119 -0.1675 0.4417 0.106 Uiso 1 1 calc R . .
H22B H 0.4944 -0.2047 0.3437 0.106 Uiso 1 1 calc R . .
H22C H 0.2880 -0.1827 0.3332 0.106 Uiso 1 1 calc R . .
C23 C 0.4981(15) -0.0511(10) 0.3693(8) 0.064(3) 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 77.4(2) . . ?
N2 Ga1 N3 77.3(2) . . ?
N1 Ga1 N3 154.6(2) . . ?
N2 Ga1 I2 120.29(15) . . ?
N1 Ga1 I2 96.75(15) . . ?
N3 Ga1 I2 97.32(15) . . ?
N2 Ga1 I1 122.34(15) . . ?
N1 Ga1 I1 97.08(15) . . ?
N3 Ga1 I1 95.11(15) . . ?
I2 Ga1 I1 117.37(4) . . ?
C1 N1 C5 118.9(6) . . ?
C1 N1 Ga1 124.5(5) . . ?
C5 N1 Ga1 116.6(4) . . ?
C6 N2 C10 121.2(5) . . ?
C6 N2 Ga1 119.2(4) . . ?
C10 N2 Ga1 119.6(4) . . ?
C15 N3 C11 119.9(6) . . ?
C15 N3 Ga1 125.1(4) . . ?
C11 N3 Ga1 114.9(4) . . ?
N1 C1 C2 121.5(6) . . ?
C1 C2 C3 119.7(6) . . ?
C2 C3 C4 119.2(7) . . ?
C5 C4 C3 118.6(6) . . ?
N1 C5 C4 122.1(5) . . ?
N1 C5 C6 112.4(6) . . ?
C4 C5 C6 125.4(6) . . ?
N2 C6 C7 120.7(6) . . ?
N2 C6 C5 114.1(5) . . ?
C7 C6 C5 125.2(6) . . ?
C6 C7 C8 119.6(6) . . ?
C9 C8 C7 117.3(6) . . ?
C9 C8 C16 121.3(5) . . ?
C7 C8 C16 121.4(6) . . ?
C10 C9 C8 120.9(6) . . ?
N2 C10 C9 120.1(6) . . ?
N2 C10 C11 114.3(5) . . ?
C9 C10 C11 125.5(6) . . ?
N3 C11 C12 121.1(6) . . ?
N3 C11 C10 113.6(5) . . ?
C12 C11 C10 125.3(6) . . ?
C11 C12 C13 118.1(6) . . ?
C14 C13 C12 120.2(7) . . ?
C13 C14 C15 119.7(7) . . ?
N3 C15 C14 120.9(6) . . ?
C21 C16 C17 117.6(6) . . ?
C21 C16 C8 121.1(6) . . ?
C17 C16 C8 121.2(6) . . ?
C18 C17 C16 121.0(6) . . ?
C17 C18 C19 120.8(7) . . ?
C20 C19 C18 118.6(6) . . ?
C19 C20 C21 121.6(6) . . ?
C20 C21 C16 120.3(6) . . ?
N4 C23 C22 179.5(13) . . ?
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 2.5389(11) . ?
I2 Ga1 2.5144(12) . ?
Ga1 N2 2.007(5) . ?
Ga1 N1 2.087(5) . ?
Ga1 N3 2.121(5) . ?
N1 C1 1.357(8) . ?
N1 C5 1.362(8) . ?
N2 C6 1.343(8) . ?
N2 C10 1.350(8) . ?
N3 C15 1.331(8) . ?
N3 C11 1.373(8) . ?
N4 C23 1.141(13) . ?
C1 C2 1.368(10) . ?
C2 C3 1.386(10) . ?
C3 C4 1.395(9) . ?
C4 C5 1.372(9) . ?
C5 C6 1.491(8) . ?
C6 C7 1.383(9) . ?
C7 C8 1.412(8) . ?
C8 C9 1.396(9) . ?
C8 C16 1.479(9) . ?
C9 C10 1.374(9) . ?
C10 C11 1.470(9) . ?
C11 C12 1.376(9) . ?
C12 C13 1.391(10) . ?
C13 C14 1.362(10) . ?
C14 C15 1.380(9) . ?
C16 C21 1.399(9) . ?
C16 C17 1.407(9) . ?
C17 C18 1.379(9) . ?
C18 C19 1.385(10) . ?
C19 C20 1.379(10) . ?
C20 C21 1.386(9) . ?
C22 C23 1.458(15) . ?
