#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/15/2011501.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2011501
loop_
_publ_author_name
'Müller, Peter'
'Usón, Isabel'
'Prust, Jörg'
'Roesky, Herbert W.'
_publ_section_title
;
 Tetrameric indium trichloride, a new modification of a widely used
 compound
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1300
_journal_page_last               1301
_journal_paper_doi               10.1107/S0108270100010362
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[In4 Cl12 (C4 H11 N)6]'
_chemical_formula_sum            'C24 H66 Cl12 In4 N6'
_chemical_formula_weight         1323.64
_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'
_cell_angle_alpha                95.46(3)
_cell_angle_beta                 109.57(3)
_cell_angle_gamma                114.20(3)
_cell_formula_units_Z            1
_cell_length_a                   10.962(2)
_cell_length_b                   11.407(2)
_cell_length_c                   11.674(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.9
_cell_volume                     1207.8(7)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XP in SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type
'Stoe-Siemens-Huber four-circle diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .046
_diffrn_reflns_av_sigmaI/netI    .018
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            45298
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  .783
_exptl_absorpt_correction_T_min  .512
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .1
_refine_diff_density_max         .58
_refine_diff_density_min         -1.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         5291
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          .026
_refine_ls_R_factor_gt           .023
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0293P)²+0.4598P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .054
_reflns_number_gt                4871
_reflns_number_total             5291
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            de1146.cif
_cod_data_source_block           I
_cod_original_cell_volume        1207.8(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2011501
_cod_database_fobs_code          2011501
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
In1 -.16254(2) .17520(2) .267270(10) .01588(5) Uani d . 1 . . In
In2 .09422(2) .422900(10) .123130(10) .01431(5) Uani d . 1 . . In
Cl1 -.15375(6) .21661(5) .03551(5) .01800(10) Uani d . 1 . . Cl
Cl2 .09098(6) .41004(5) .33569(5) .01800(10) Uani d . 1 . . Cl
Cl3 -.37922(7) -.03459(6) .15741(6) .02790(10) Uani d . 1 . . Cl
Cl4 -.12865(7) .19437(6) .48348(5) .02710(10) Uani d . 1 . . Cl
Cl5 .22419(7) .29472(6) .13154(6) .02270(10) Uani d . 1 . . Cl
Cl6 .05579(6) .44214(5) -.10137(5) .01690(10) Uani d . 1 . . Cl
N1 -.2675(2) .3108(2) .2337(2) .0178(4) Uani d D 1 . . N
H1 -.232(3) .350(2) .182(2) .021 Uiso d D 1 . . H
C1 -.2138(3) .4232(2) .3454(2) .0266(5) Uani d . 1 . . C
H11 -.1053 .4726 .3810 .032 Uiso calc R 1 . . H
H12 -.2422 .3858 .4111 .032 Uiso calc R 1 . . H
C2 -.2742(3) .5203(3) .3138(3) .0320(6) Uani d . 1 . . C
H21 -.2561 .5503 .2424 .048 Uiso calc R 1 . . H
H22 -.2254 .5975 .3873 .048 Uiso calc R 1 . . H
H23 -.3800 .4757 .2913 .048 Uiso calc R 1 . . H
C3 -.4310(3) .2349(2) .1691(2) .0245(5) Uani d . 1 . . C
H31 -.4597 .1613 .0972 .029 Uiso calc R 1 . . H
H32 -.4691 .2950 .1348 .029 Uiso calc R 1 . . H
C4 -.5005(3) .1773(3) .2570(3) .0382(7) Uani d . 1 . . C
H41 -.4486 .1333 .3048 .057 Uiso calc R 1 . . H
H42 -.6039 .1120 .2072 .057 Uiso calc R 1 . . H
H43 -.4939 .2493 .3156 .057 Uiso calc R 1 . . H
N2 .0003(2) .1031(2) .2658(2) .0181(4) Uani d D 1 . . N
H2 .054(3) .163(2) .237(2) .022 Uiso d D 1 . . H
C5 .1007(3) .1161(2) .3956(2) .0225(5) Uani d . 1 . . C
H51 .0477 .0417 .4264 .027 Uiso calc R 1 . . H
H52 .1265 .2005 .4528 .027 Uiso calc R 1 . . H
C6 .2404(3) .1151(3) .4029(3) .0387(7) Uani d . 1 . . C
H61 .2162 .0307 .3487 .058 Uiso calc R 1 . . H
H62 .3009 .1245 .4903 .058 Uiso calc R 1 . . H
H63 .2949 .1896 .3743 .058 Uiso calc R 1 . . H
C7 -.0581(3) -.0279(2) .1726(2) .0259(5) Uani d . 1 . . C
H71 .0221 -.0284 .1517 .031 Uiso calc R 1 . . H
H72 -.1358 -.0351 .0938 .031 Uiso calc R 1 . . H
C8 -.1206(3) -.1487(3) .2196(3) .0339(6) Uani d . 1 . . C
H81 -.0406 -.1528 .2862 .051 Uiso calc R 1 . . H
H82 -.1731 -.2298 .1496 .051 Uiso calc R 1 . . H
H83 -.1886 -.1416 .2536 .051 Uiso calc R 1 . . H
N3 .2885(2) .6302(2) .2043(2) .0164(4) Uani d D 1 . . N
H3 .270(3) .675(2) .148(2) .020 Uiso d D 1 . . H
C9 .3011(3) .7068(2) .3231(2) .0200(5) Uani d . 1 . . C
H91 .3580 .6859 .3963 .024 Uiso calc R 1 . . H
H92 .2017 .6776 .3209 .024 Uiso calc R 1 . . H
C10 .3748(3) .8562(2) .3411(2) .0281(5) Uani d . 1 . . C
H101 .4747 .8864 .3466 .042 Uiso calc R 1 . . H
H102 .3789 .9012 .4191 .042 Uiso calc R 1 . . H
H103 .3186 .8777 .2693 .042 Uiso calc R 1 . . H
C11 .4325(3) .6367(2) .2198(2) .0217(5) Uani d . 1 . . C
H111 .4472 .5719 .2661 .026 Uiso calc R 1 . . H
H112 .5126 .7270 .2713 .026 Uiso calc R 1 . . H
C12 .4415(3) .6067(2) .0953(2) .0252(5) Uani d . 1 . . C
H121 .3676 .5147 .0468 .038 Uiso calc R 1 . . H
H122 .5395 .6173 .1105 .038 Uiso calc R 1 . . H
H123 .4234 .6684 .0477 .038 Uiso calc R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -.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_site_symmetry_3
_geom_angle
N2 In1 N1 . 155.12(7)
N2 In1 Cl3 . 96.92(6)
N1 In1 Cl3 . 98.42(6)
N2 In1 Cl4 . 99.63(6)
N1 In1 Cl4 . 95.84(6)
Cl3 In1 Cl4 . 103.04(5)
N2 In1 Cl2 . 77.64(5)
N1 In1 Cl2 . 82.72(5)
Cl3 In1 Cl2 . 165.53(2)
Cl4 In1 Cl2 . 91.14(5)
N2 In1 Cl1 . 81.63(5)
N1 In1 Cl1 . 78.90(5)
Cl3 In1 Cl1 . 90.04(4)
Cl4 In1 Cl1 . 166.54(2)
Cl2 In1 Cl1 . 75.97(4)
N3 In2 Cl5 . 98.95(5)
N3 In2 Cl2 . 92.15(6)
Cl5 In2 Cl2 . 93.45(3)
N3 In2 Cl1 . 167.85(5)
Cl5 In2 Cl1 . 93.10(3)
Cl2 In2 Cl1 . 85.54(4)
N3 In2 Cl6 . 90.70(6)
Cl5 In2 Cl6 . 96.15(3)
Cl2 In2 Cl6 . 169.43(2)
Cl1 In2 Cl6 . 89.54(5)
N3 In2 Cl6 2_565 82.61(5)
Cl5 In2 Cl6 2_565 177.08(2)
Cl2 In2 Cl6 2_565 88.95(3)
Cl1 In2 Cl6 2_565 85.42(3)
Cl6 In2 Cl6 2_565 81.33(3)
In2 Cl1 In1 . 97.88(4)
In2 Cl2 In1 . 100.24(5)
In2 Cl6 In2 2_565 98.67(3)
C3 N1 C1 . 112.8(2)
C3 N1 In1 . 112.60(10)
C1 N1 In1 . 115.50(10)
N1 C1 C2 . 113.3(2)
N1 C3 C4 . 112.5(2)
C5 N2 C7 . 113.7(2)
C5 N2 In1 . 112.60(10)
C7 N2 In1 . 117.0(2)
N2 C5 C6 . 113.9(2)
N2 C7 C8 . 113.9(2)
C11 N3 C9 . 110.9(2)
C11 N3 In2 . 115.10(10)
C9 N3 In2 . 113.50(10)
N3 C9 C10 . 112.8(2)
N3 C11 C12 . 112.6(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
In1 N2 . 2.256(2) ?
In1 N1 . 2.267(2) ?
In1 Cl3 . 2.394(2) ?
In1 Cl4 . 2.3994(8) ?
In1 Cl2 . 2.746(2) ?
In1 Cl1 . 2.8165(8) ?
In2 N3 . 2.263(2) ?
In2 Cl5 . 2.4122(8) ?
In2 Cl2 . 2.5109(7) ?
In2 Cl1 . 2.531(2) ?
In2 Cl6 . 2.5573(8) ?
In2 Cl6 2_565 2.6474(8) ?
Cl6 In2 2_565 2.6474(8) ?
N1 C3 . 1.493(3) ?
N1 C1 . 1.498(3) ?
C1 C2 . 1.522(3) ?
C3 C4 . 1.519(4) ?
N2 C5 . 1.496(3) ?
N2 C7 . 1.505(3) ?
C5 C6 . 1.510(3) ?
C7 C8 . 1.514(4) ?
N3 C11 . 1.497(3) ?
N3 C9 . 1.499(3) ?
C9 C10 . 1.513(3) ?
C11 C12 . 1.506(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1 Cl1 . .88(2) 2.75(2) 3.258(2) 118(2)
N2 H2 Cl5 . .88(2) 2.62(2) 3.476(2) 167(2)
N2 H2 Cl2 . .88(2) 2.76(2) 3.158(2) 110(2)
N1 H1 Cl6 2_565 .88(2) 2.85(2) 3.685(2) 158(2)
N3 H3 Cl1 2_565 .89(2) 2.78(2) 3.653(2) 168(2)
