#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:25:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180138 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/35/7103594.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_7103594
loop_
_publ_author_name
'Green, Shaun P'
'Jones, Cameron'
'Stasch, Andreas'
_publ_section_title
;
 Synthesis and structural characterisation of a soluble, metastable
 indium(I) halide complex, [InBr(tmeda)].
;
_journal_issue                   47
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6285
_journal_page_last               6287
_journal_paper_doi               10.1039/b814658f
_journal_year                    2008
_chemical_formula_sum            'C12 H32 Br4 In2 N4'
_chemical_formula_weight         781.70
_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                   17.327(4)
_cell_length_b                   12.110(2)
_cell_length_c                   22.420(5)
_cell_measurement_temperature    123(2)
_cell_volume                     4704.4(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1382
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32336
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    8.757
_exptl_absorpt_correction_T_max  0.353
_exptl_absorpt_correction_T_min  0.261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.705
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4317
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0552
_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)+(0.0732P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1493
_reflns_number_gt                2539
_reflns_number_total             4317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b814658f.txt
_cod_data_source_block           '[In2Br4(tmeda)2]'
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7103594
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 0.06494(4) 0.21178(6) 0.35853(3) 0.0261(2) Uani 1 1 d . . .
In2 In -0.07530(4) 0.28265(6) 0.40269(3) 0.0278(2) Uani 1 1 d . . .
Br1 Br 0.01638(7) 0.00028(9) 0.34276(5) 0.0384(3) Uani 1 1 d . . .
Br2 Br 0.18490(6) 0.14822(10) 0.41700(6) 0.0420(4) Uani 1 1 d . . .
Br3 Br -0.13388(7) 0.32065(11) 0.29266(5) 0.0479(4) Uani 1 1 d . . .
Br4 Br -0.11122(7) 0.47552(10) 0.44083(6) 0.0446(4) Uani 1 1 d . . .
N1 N 0.1113(5) 0.2082(8) 0.2612(4) 0.040(3) Uani 1 1 d . . .
N2 N 0.1256(5) 0.3919(7) 0.3452(4) 0.031(2) Uani 1 1 d . . .
N3 N -0.1843(5) 0.1740(8) 0.4217(4) 0.034(2) Uani 1 1 d D . .
N4 N -0.0586(4) 0.2194(7) 0.5070(4) 0.024(2) Uani 1 1 d D . .
C1 C 0.0507(8) 0.1786(11) 0.2194(5) 0.055(4) Uani 1 1 d . . .
H1A H 0.0715 0.1780 0.1788 0.082 Uiso 1 1 calc R . .
H1B H 0.0087 0.2327 0.2220 0.082 Uiso 1 1 calc R . .
H1C H 0.0308 0.1050 0.2293 0.082 Uiso 1 1 calc R . .
C2 C 0.1730(7) 0.1223(10) 0.2576(6) 0.053(4) Uani 1 1 d . . .
H2A H 0.1539 0.0531 0.2747 0.080 Uiso 1 1 calc R . .
H2B H 0.2185 0.1472 0.2798 0.080 Uiso 1 1 calc R . .
H2C H 0.1871 0.1103 0.2157 0.080 Uiso 1 1 calc R . .
C3 C 0.1441(8) 0.3190(9) 0.2450(5) 0.050(4) Uani 1 1 d . . .
H3A H 0.1831 0.3095 0.2132 0.060 Uiso 1 1 calc R . .
H3B H 0.1023 0.3663 0.2290 0.060 Uiso 1 1 calc R . .
C4 C 0.1805(7) 0.3754(10) 0.2970(6) 0.052(4) Uani 1 1 d . . .
H4A H 0.2242 0.3303 0.3117 0.062 Uiso 1 1 calc R . .
H4B H 0.2011 0.4479 0.2842 0.062 Uiso 1 1 calc R . .
C5 C 0.1658(7) 0.4337(11) 0.3999(6) 0.052(4) Uani 1 1 d . . .
H5A H 0.2063 0.3815 0.4116 0.078 Uiso 1 1 calc R . .
H5B H 0.1284 0.4409 0.4325 0.078 Uiso 1 1 calc R . .
H5C H 0.1889 0.5058 0.3915 0.078 Uiso 1 1 calc R . .
C6 C 0.0658(6) 0.4735(9) 0.3292(6) 0.052(4) Uani 1 1 d . . .
H6A H 0.0905 0.5431 0.3177 0.079 Uiso 1 1 calc R . .
H6B H 0.0320 0.4862 0.3636 0.079 Uiso 1 1 calc R . .
H6C H 0.0352 0.4454 0.2957 0.079 Uiso 1 1 calc R . .
C7 C -0.1869(6) 0.0834(10) 0.3777(6) 0.042(3) Uani 1 1 d . . .
H7A H -0.2300 0.0339 0.3871 0.064 Uiso 1 1 calc R . .
H7B H -0.1384 0.0419 0.3791 0.064 Uiso 1 1 calc R . .
H7C H -0.1941 0.1142 0.3376 0.064 Uiso 1 1 calc R . .
C8 C -0.2540(6) 0.2422(11) 0.4163(5) 0.049(4) Uani 1 1 d . . .
H8A H -0.2593 0.2678 0.3750 0.074 Uiso 1 1 calc R . .
H8B H -0.2498 0.3060 0.4430 0.074 Uiso 1 1 calc R . .
H8C H -0.2993 0.1983 0.4273 0.074 Uiso 1 1 calc R . .
C9 C -0.1819(6) 0.1305(12) 0.4837(5) 0.059(4) Uani 1 1 d DU . .
H9A H -0.2062 0.0565 0.4841 0.071 Uiso 1 1 calc R . .
H9B H -0.2136 0.1794 0.5094 0.071 Uiso 1 1 calc R . .
C10 C -0.1030(7) 0.1213(13) 0.5106(7) 0.095(5) Uani 1 1 d DU . .
H10A H -0.1083 0.1002 0.5531 0.113 Uiso 1 1 calc R . .
H10B H -0.0746 0.0612 0.4901 0.113 Uiso 1 1 calc R . .
C11 C -0.0714(9) 0.2967(12) 0.5549(7) 0.076(5) Uani 1 1 d U . .
H11A H -0.0636 0.2595 0.5932 0.113 Uiso 1 1 calc R . .
H11B H -0.1244 0.3248 0.5527 0.113 Uiso 1 1 calc R . .
H11C H -0.0351 0.3583 0.5513 0.113 Uiso 1 1 calc R . .
C12 C 0.0211(9) 0.1790(13) 0.5140(7) 0.083(5) Uani 1 1 d U . .
H12A H 0.0249 0.1346 0.5504 0.124 Uiso 1 1 calc R . .
H12B H 0.0564 0.2420 0.5167 0.124 Uiso 1 1 calc R . .
H12C H 0.0350 0.1335 0.4795 0.124 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'
Br Br -0.2901 2.4595 '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'
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 75.7(3) . . ?
N1 In1 Br2 101.1(3) . . ?
N2 In1 Br2 89.0(2) . . ?
N1 In1 Br1 88.1(2) . . ?
N2 In1 Br1 163.7(2) . . ?
Br2 In1 Br1 91.97(5) . . ?
N1 In1 In2 130.3(3) . . ?
N2 In1 In2 98.34(19) . . ?
Br2 In1 In2 128.37(5) . . ?
Br1 In1 In2 93.84(4) . . ?
N3 In2 N4 75.4(3) . . ?
N3 In2 Br4 104.8(2) . . ?
N4 In2 Br4 89.72(19) . . ?
N3 In2 Br3 87.7(2) . . ?
N4 In2 Br3 163.03(18) . . ?
Br4 In2 Br3 93.32(5) . . ?
N3 In2 In1 126.9(2) . . ?
N4 In2 In1 98.03(18) . . ?
Br4 In2 In1 128.06(4) . . ?
Br3 In2 In1 93.21(4) . . ?
C1 N1 C2 108.1(10) . . ?
C1 N1 C3 109.8(10) . . ?
C2 N1 C3 109.8(9) . . ?
C1 N1 In1 111.0(7) . . ?
C2 N1 In1 108.1(7) . . ?
C3 N1 In1 109.9(7) . . ?
C4 N2 C6 111.8(10) . . ?
C4 N2 C5 110.5(9) . . ?
C6 N2 C5 107.4(9) . . ?
C4 N2 In1 104.5(6) . . ?
C6 N2 In1 109.1(6) . . ?
C5 N2 In1 113.6(7) . . ?
C8 N3 C7 109.7(9) . . ?
C8 N3 C9 107.4(9) . . ?
C7 N3 C9 111.3(10) . . ?
C8 N3 In2 109.4(7) . . ?
C7 N3 In2 108.7(6) . . ?
C9 N3 In2 110.3(6) . . ?
C10 N4 C11 114.7(11) . . ?
C10 N4 C12 102.9(10) . . ?
C11 N4 C12 106.3(10) . . ?
C10 N4 In2 104.4(7) . . ?
C11 N4 In2 119.0(8) . . ?
C12 N4 In2 108.2(7) . . ?
C4 C3 N1 112.3(10) . . ?
N2 C4 C3 111.5(9) . . ?
N3 C9 C10 115.3(10) . . ?
N4 C10 C9 114.1(11) . . ?
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 2.326(9) . ?
In1 N2 2.440(8) . ?
In1 Br2 2.5752(14) . ?
In1 Br1 2.7190(14) . ?
In1 In2 2.7608(11) . ?
In2 N3 2.341(8) . ?
In2 N4 2.478(8) . ?
In2 Br4 2.5639(14) . ?
In2 Br3 2.7070(14) . ?
N1 C1 1.453(15) . ?
N1 C2 1.493(14) . ?
N1 C3 1.501(14) . ?
N2 C4 1.453(13) . ?
N2 C6 1.475(13) . ?
N2 C5 1.499(14) . ?
N3 C8 1.468(14) . ?
N3 C7 1.477(15) . ?
N3 C9 1.487(12) . ?
N4 C10 1.417(13) . ?
N4 C11 1.441(16) . ?
N4 C12 1.473(16) . ?
C3 C4 1.492(16) . ?
C9 C10 1.500(9) . ?
