#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:02:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180056 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/02/7050211.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_7050211
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            'C22 H30 Cl3 In N2 O'
_chemical_formula_weight         559.65
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.008(3)
_cell_length_b                   16.621(3)
_cell_length_c                   17.465(4)
_cell_measurement_temperature    150(2)
_cell_volume                     4937.2(17)
_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  0.1004
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23141
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0463
_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)+(0.0276P)²+10.5774P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                3158
_reflns_number_total             4490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b310592j.txt
_cod_data_source_block           compound_7
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7050211
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
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
In1 In 0.087112(19) 0.134843(19) 0.301961(19) 0.01814(12) Uani 1 1 d . . .
Cl1 Cl 0.18988(7) 0.13312(8) 0.20465(7) 0.0273(3) Uani 1 1 d . . .
Cl2 Cl 0.16583(7) 0.14080(8) 0.41658(7) 0.0249(3) Uani 1 1 d . . .
Cl3 Cl 0.05748(7) -0.00873(7) 0.29696(9) 0.0312(3) Uani 1 1 d . . .
O1 O -0.02206(19) 0.1407(2) 0.38847(19) 0.0251(8) Uani 1 1 d . . .
N1 N -0.0170(2) 0.1642(2) 0.2221(2) 0.0196(9) Uani 1 1 d . . .
N2 N 0.0746(2) 0.2753(2) 0.2944(2) 0.0163(9) Uani 1 1 d . . .
C1 C -0.0665(3) 0.1108(3) 0.1911(3) 0.0271(12) Uani 1 1 d . . .
H1 H -0.0554 0.0562 0.1959 0.032 Uiso 1 1 calc R . .
C2 C -0.1337(3) 0.1338(3) 0.1523(3) 0.0277(12) Uani 1 1 d . . .
H2 H -0.1669 0.0952 0.1313 0.033 Uiso 1 1 calc R . .
C3 C -0.1512(3) 0.2139(3) 0.1449(3) 0.0267(12) Uani 1 1 d . . .
H3 H -0.1969 0.2303 0.1202 0.032 Uiso 1 1 calc R . .
C4 C -0.0993(3) 0.2698(3) 0.1748(3) 0.0217(11) Uani 1 1 d . . .
H4 H -0.1087 0.3245 0.1691 0.026 Uiso 1 1 calc R . .
C5 C -0.0331(2) 0.2431(3) 0.2135(3) 0.0147(10) Uani 1 1 d . . .
C6 C 0.0206(3) 0.2999(3) 0.2497(3) 0.0182(11) Uani 1 1 d . . .
H6 H 0.0154 0.3547 0.2400 0.022 Uiso 1 1 calc R . .
C7 C 0.1290(3) 0.3341(3) 0.3253(3) 0.0187(11) Uani 1 1 d . . .
C8 C 0.1226(3) 0.3528(3) 0.4038(3) 0.0206(11) Uani 1 1 d . . .
C9 C 0.1769(3) 0.4074(3) 0.4336(3) 0.0300(13) Uani 1 1 d . . .
H9 H 0.1750 0.4203 0.4854 0.036 Uiso 1 1 calc R . .
C10 C 0.2328(3) 0.4423(3) 0.3883(3) 0.0322(14) Uani 1 1 d . . .
H10 H 0.2685 0.4782 0.4098 0.039 Uiso 1 1 calc R . .
C11 C 0.2370(3) 0.4249(3) 0.3110(3) 0.0302(13) Uani 1 1 d . . .
H11 H 0.2753 0.4496 0.2811 0.036 Uiso 1 1 calc R . .
C12 C 0.1845(3) 0.3707(3) 0.2768(3) 0.0222(11) Uani 1 1 d . . .
C13 C 0.0546(3) 0.3208(3) 0.4510(3) 0.0309(13) Uani 1 1 d . . .
H13 H 0.0378 0.2698 0.4281 0.037 Uiso 1 1 calc R . .
C14 C -0.0140(3) 0.3794(4) 0.4456(4) 0.0477(17) Uani 1 1 d . . .
H14A H 0.0014 0.4304 0.4667 0.072 Uiso 1 1 calc R . .
H14B H -0.0579 0.3586 0.4739 0.072 Uiso 1 1 calc R . .
H14C H -0.0286 0.3863 0.3930 0.072 Uiso 1 1 calc R . .
C15 C 0.0757(4) 0.3045(4) 0.5342(3) 0.0534(19) Uani 1 1 d . . .
H15A H 0.1214 0.2706 0.5364 0.080 Uiso 1 1 calc R . .
H15B H 0.0325 0.2782 0.5592 0.080 Uiso 1 1 calc R . .
H15C H 0.0867 0.3545 0.5596 0.080 Uiso 1 1 calc R . .
C16 C 0.1889(3) 0.3561(3) 0.1911(3) 0.0267(12) Uani 1 1 d . . .
H16 H 0.1546 0.3106 0.1790 0.032 Uiso 1 1 calc R . .
C17 C 0.1590(3) 0.4299(3) 0.1465(3) 0.0382(15) Uani 1 1 d . . .
H17A H 0.1917 0.4755 0.1577 0.057 Uiso 1 1 calc R . .
H17B H 0.1058 0.4415 0.1613 0.057 Uiso 1 1 calc R . .
H17C H 0.1607 0.4188 0.0925 0.057 Uiso 1 1 calc R . .
C18 C 0.2729(3) 0.3344(4) 0.1652(4) 0.0397(15) Uani 1 1 d . . .
H18A H 0.3077 0.3784 0.1760 0.060 Uiso 1 1 calc R . .
H18B H 0.2730 0.3238 0.1111 0.060 Uiso 1 1 calc R . .
H18C H 0.2904 0.2874 0.1922 0.060 Uiso 1 1 calc R . .
C19 C -0.0189(3) 0.0941(4) 0.4594(3) 0.0414(16) Uani 1 1 d . . .
H19A H 0.0172 0.1187 0.4955 0.050 Uiso 1 1 calc R . .
H19B H -0.0016 0.0396 0.4492 0.050 Uiso 1 1 calc R . .
C20 C -0.1000(3) 0.0941(4) 0.4907(3) 0.0406(15) Uani 1 1 d . . .
H20A H -0.0991 0.0963 0.5462 0.049 Uiso 1 1 calc R . .
H20B H -0.1282 0.0462 0.4749 0.049 Uiso 1 1 calc R . .
C21 C -0.1374(3) 0.1681(4) 0.4581(3) 0.0391(15) Uani 1 1 d . . .
H21A H -0.1264 0.2149 0.4896 0.047 Uiso 1 1 calc R . .
H21B H -0.1939 0.1616 0.4537 0.047 Uiso 1 1 calc R . .
C22 C -0.0998(3) 0.1757(4) 0.3806(3) 0.0309(13) Uani 1 1 d . . .
H22A H -0.1302 0.1470 0.3424 0.037 Uiso 1 1 calc R . .
H22B H -0.0962 0.2318 0.3656 0.037 Uiso 1 1 calc R . .
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'
In In -0.7276 1.3100 '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'
O O 0.0106 0.0060 '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
N1 In1 N2 71.72(13) . . ?
N1 In1 O1 77.16(12) . . ?
N2 In1 O1 85.69(12) . . ?
N1 In1 Cl2 156.94(10) . . ?
N2 In1 Cl2 93.21(10) . . ?
O1 In1 Cl2 84.55(9) . . ?
N1 In1 Cl1 97.54(10) . . ?
N2 In1 Cl1 92.14(10) . . ?
O1 In1 Cl1 174.67(8) . . ?
Cl2 In1 Cl1 100.44(5) . . ?
N1 In1 Cl3 91.53(10) . . ?
N2 In1 Cl3 162.10(9) . . ?
O1 In1 Cl3 84.39(9) . . ?
Cl2 In1 Cl3 100.63(5) . . ?
Cl1 In1 Cl3 96.41(5) . . ?
C22 O1 C19 109.0(4) . . ?
C22 O1 In1 131.5(3) . . ?
C19 O1 In1 119.0(3) . . ?
C1 N1 C5 118.2(4) . . ?
C1 N1 In1 126.0(3) . . ?
C5 N1 In1 115.4(3) . . ?
C6 N2 C7 118.1(4) . . ?
C6 N2 In1 114.8(3) . . ?
C7 N2 In1 126.4(3) . . ?
N1 C1 C2 122.3(5) . . ?
C3 C2 C1 119.7(5) . . ?
C2 C3 C4 118.6(5) . . ?
C5 C4 C3 119.2(5) . . ?
N1 C5 C4 122.1(4) . . ?
N1 C5 C6 117.0(4) . . ?
C4 C5 C6 120.9(4) . . ?
N2 C6 C5 120.6(4) . . ?
C12 C7 C8 122.8(5) . . ?
C12 C7 N2 119.8(4) . . ?
C8 C7 N2 117.5(4) . . ?
C9 C8 C7 117.1(5) . . ?
C9 C8 C13 122.0(5) . . ?
C7 C8 C13 120.6(4) . . ?
C10 C9 C8 121.4(5) . . ?
C9 C10 C11 120.8(5) . . ?
C10 C11 C12 121.2(5) . . ?
C11 C12 C7 116.7(5) . . ?
C11 C12 C16 119.4(5) . . ?
C7 C12 C16 123.9(4) . . ?
C8 C13 C15 113.7(5) . . ?
C8 C13 C14 109.0(4) . . ?
C15 C13 C14 110.7(5) . . ?
C12 C16 C17 110.9(4) . . ?
C12 C16 C18 111.9(5) . . ?
C17 C16 C18 110.1(4) . . ?
O1 C19 C20 106.2(4) . . ?
C19 C20 C21 104.8(5) . . ?
C20 C21 C22 103.3(4) . . ?
O1 C22 C21 105.6(4) . . ?
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
In1 N1 2.306(4) . ?
In1 N2 2.348(4) . ?
In1 O1 2.396(3) . ?
In1 Cl2 2.4103(13) . ?
In1 Cl1 2.4381(13) . ?
In1 Cl3 2.4405(13) . ?
O1 C22 1.452(6) . ?
O1 C19 1.462(6) . ?
N1 C1 1.339(6) . ?
N1 C5 1.348(6) . ?
N2 C6 1.273(6) . ?
N2 C7 1.449(6) . ?
C1 C2 1.383(7) . ?
C2 C3 1.369(7) . ?
C3 C4 1.384(7) . ?
C4 C5 1.386(6) . ?
C5 C6 1.458(6) . ?
C7 C12 1.406(7) . ?
C7 C8 1.411(7) . ?
C8 C9 1.395(7) . ?
C8 C13 1.516(7) . ?
C9 C10 1.366(8) . ?
C10 C11 1.383(8) . ?
C11 C12 1.401(7) . ?
C12 C16 1.518(7) . ?
C13 C15 1.522(8) . ?
C13 C14 1.523(8) . ?
C16 C17 1.541(7) . ?
C16 C18 1.542(7) . ?
C19 C20 1.483(8) . ?
C20 C21 1.498(8) . ?
C21 C22 1.502(7) . ?
