Structures and Stability of Molecular InBr3Pyx (x= 1-3) Complexes: Unexpected Solid State Stabilization of Dimeric In2Br6Py4As Compared to Valence-Isoelectronic Group 15 and 17 Halogen Bridging Dimers
Igor V. Kazakov; Michael Bodensteiner; Anna S. Lisovenko; Andrew V. Suvorov; Manfred Scheer; Gábor Balázs; Alexey Y. Timoshkin; Inorganic Chemistry 52 (2013) 13207–13215; doi:10.1021/ic402162d

data_4336764
_publ_contact_author_name
;
;
_publ_section_title
;
 Structures and Stability of Molecular InBr3Pyx (x= 1-3) Complexes:
 Unexpected Solid State Stabilization of Dimeric In2Br6Py4As Compared to
 Valence-Isoelectronic Group 15 and 17 Halogen Bridging Dimers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13207
_journal_page_last               13215
_journal_paper_doi               10.1021/ic402162d
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'Cl6 I2'
_chemical_formula_sum            'Cl6 I2'
_chemical_formula_weight         466.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-08-21
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                71.756(5)
_cell_angle_beta                 78.314(5)
_cell_angle_gamma                81.092(5)
_cell_formula_units_Z            1
_cell_length_a                   5.4020(3)
_cell_length_b                   5.6323(3)
_cell_length_c                   8.3070(4)
_cell_measurement_reflns_used    4806
_cell_measurement_temperature    123.05(10)
_cell_measurement_theta_max      34.6450
_cell_measurement_theta_min      3.8180
_cell_volume                     233.93(2)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      123.05(10)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9583
_diffrn_measurement_details
;
  1 omega  -99.00  -42.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1591  -38.0000  -60.0000 57

  2 omega  -21.00   43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1591   38.0000  120.0000 64

  3 omega -101.00    8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1591  -77.0000 -120.0000 109

  4 omega -101.00    5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1591  -77.0000   30.0000 106

  5 omega   -1.00   62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.2528  -99.0000 -180.0000 63

  6 omega  -99.00    4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1591  -57.0000   90.0000 103

  7 omega  -50.00   51.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1591   38.0000 -120.0000 101

  8 omega  -50.00   51.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1591   38.0000    0.0000 101

  9 omega -101.00    1.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1591  -38.0000 -180.0000 102

 10 omega   57.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.2528  178.0000 -180.0000 59

 11 omega   53.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.2528 -178.0000   90.0000 62

 12 omega   -3.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.2528   57.0000    0.0000 103

 13 omega   -4.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.2528  -99.0000 -120.0000 72

 14 omega -115.00  -35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1591 -178.0000  -30.0000 80

 15 omega   -7.00   62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.2528   77.0000   90.0000 69
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0789586000
_diffrn_orient_matrix_UB_12      0.0791768000
_diffrn_orient_matrix_UB_13      0.0135229000
_diffrn_orient_matrix_UB_21      -0.0670937000
_diffrn_orient_matrix_UB_22      -0.0164523000
_diffrn_orient_matrix_UB_23      0.0848826000
_diffrn_orient_matrix_UB_31      0.0861269000
_diffrn_orient_matrix_UB_32      -0.1058986000
_diffrn_orient_matrix_UB_33      0.0303140000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9677
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.964
_diffrn_reflns_theta_min         3.828
_diffrn_source                   'Enhance (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    8.348
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.298
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.311
_exptl_crystal_description       block
_exptl_crystal_F_000             208
_exptl_crystal_size_max          0.2731
_exptl_crystal_size_mid          0.1022
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.322
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         1975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0144P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_ref         0.0372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1727
_reflns_number_total             1975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402162d_si_005.cif
_cod_data_source_block           absabs
_cod_database_code               4336764
_chemical_oxdiff_formula         'I2 Cl6'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_olex2_refinement_description
;
;
_shelxl_version_number           2013-2