#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/22/2212205.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_2212205
loop_
_publ_author_name
'Kochel, Andrzej'
_publ_section_title
;
 Bis(tetraphenylarsonium) hexabromorhenate(IV)
;
_journal_coeditor_code           HB2271
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m596
_journal_page_last               m597
_journal_paper_doi               10.1107/S1600536807003662
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C24 H20 As)2 [Re1 Br6]'
_chemical_formula_moiety         '2(C24 H20 As +), Br6 Re 2-'
_chemical_formula_sum            'C48 H40 As2 Br6 Re'
_chemical_formula_weight         1432.25
_chemical_name_systematic
;
Bis(tetraphenylarsonium) hexabromorhenate(IV)
;
_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
_cell_angle_alpha                92.565(7)
_cell_angle_beta                 99.915(7)
_cell_angle_gamma                116.880(9)
_cell_formula_units_Z            1
_cell_length_a                   10.4085(9)
_cell_length_b                   10.4157(9)
_cell_length_c                   12.1694(9)
_cell_measurement_reflns_used    2876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.98
_cell_volume                     1147.8(2)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2004)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2004)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Kuma KM-4-CCD'
_diffrn_measurement_method       ω
_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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0847
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9761
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    9.332
_exptl_absorpt_correction_T_max  0.598
_exptl_absorpt_correction_T_min  0.318
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2004)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.072
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             679
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.982
_refine_diff_density_min         -1.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0343
_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)+(0.0254P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                2979
_reflns_number_total             4040
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2271.cif
_cod_data_source_block           I
_cod_original_cell_volume        1147.85(16)
_cod_database_code               2212205
_cod_database_fobs_code          2212205
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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
As As1 0.32040(7) 0.38983(7) 0.18172(5) 0.01200(17) Uani d . 1
C C1 0.3148(7) 0.2496(7) 0.0703(5) 0.0123(14) Uani d . 1
C C2 0.4456(7) 0.2440(7) 0.0635(5) 0.0145(15) Uani d . 1
H H2 0.5339 0.3050 0.1136 0.017 Uiso calc R 1
C C3 0.4397(7) 0.1451(8) -0.0199(6) 0.0205(16) Uani d . 1
H H3 0.5252 0.1398 -0.0257 0.025 Uiso calc R 1
C C4 0.3097(7) 0.0551(7) -0.0939(6) 0.0194(16) Uani d . 1
H H4 0.3085 -0.0079 -0.1510 0.023 Uiso calc R 1
C C5 0.1797(7) 0.0573(7) -0.0842(6) 0.0200(17) Uani d . 1
H H5 0.0911 -0.0071 -0.1326 0.024 Uiso calc R 1
C C6 0.1829(7) 0.1561(7) -0.0019(6) 0.0191(16) Uani d . 1
H H6 0.0966 0.1592 0.0045 0.023 Uiso calc R 1
C C7 0.1753(6) 0.2831(7) 0.2665(5) 0.0117(15) Uani d . 1
C C8 0.1737(7) 0.1609(8) 0.3060(5) 0.0175(16) Uani d . 1
H H8 0.2465 0.1356 0.2967 0.021 Uiso calc R 1
C C9 0.0636(7) 0.0756(8) 0.3597(5) 0.0177(16) Uani d . 1
H H9 0.0638 -0.0060 0.3876 0.021 Uiso calc R 1
C C10 -0.0475(7) 0.1114(8) 0.3720(5) 0.0155(16) Uani d . 1
H H10 -0.1230 0.0527 0.4061 0.019 Uiso calc R 1
C C11 -0.0439(7) 0.2363(8) 0.3325(5) 0.0208(17) Uani d . 1
H H11 -0.1167 0.2620 0.3411 0.025 Uiso calc R 1
C C12 0.0679(7) 0.3220(7) 0.2807(5) 0.0146(15) Uani d . 1
H H12 0.0708 0.4060 0.2553 0.018 Uiso calc R 1
C C13 0.2637(6) 0.5190(7) 0.1055(5) 0.0146(15) Uani d . 1
C C14 0.2138(6) 0.4939(7) -0.0097(5) 0.0153(16) Uani d . 1
H H14 0.2136 0.4169 -0.0516 0.018 Uiso calc R 1
C C15 0.1639(7) 0.5827(7) -0.0636(6) 0.0180(16) Uani d . 1
H H15 0.1293 0.5652 -0.1413 0.022 Uiso calc R 1
C C16 0.1666(7) 0.6983(8) 0.0005(6) 0.0224(17) Uani d . 1
H H16 0.1322 0.7576 -0.0349 0.027 Uiso calc R 1
C C17 0.2193(7) 0.7266(7) 0.1153(6) 0.0185(16) Uani d . 1
H H17 0.2206 0.8046 0.1568 0.022 Uiso calc R 1
C C18 0.2703(7) 0.6388(7) 0.1690(6) 0.0173(16) Uani d . 1
H H18 0.3085 0.6589 0.2463 0.021 Uiso calc R 1
C C19 0.5169(7) 0.4923(7) 0.2704(5) 0.0143(15) Uani d . 1
C C20 0.5544(7) 0.4442(7) 0.3698(5) 0.0166(15) Uani d . 1
H H20 0.4820 0.3714 0.3987 0.020 Uiso calc R 1
C C21 0.7013(7) 0.5064(8) 0.4251(6) 0.0247(18) Uani d . 1
H H21 0.7282 0.4736 0.4906 0.030 Uiso calc R 1
C C22 0.8081(8) 0.6172(8) 0.3830(6) 0.0254(18) Uani d . 1
H H22 0.9067 0.6585 0.4200 0.031 Uiso calc R 1
C C23 0.7681(7) 0.6657(8) 0.2867(6) 0.0200(16) Uani d . 1
H H23 0.8396 0.7418 0.2597 0.024 Uiso calc R 1
C C24 0.6218(7) 0.6023(7) 0.2293(6) 0.0174(16) Uani d . 1
H H24 0.5955 0.6346 0.1633 0.021 Uiso calc R 1
Re Re1 0.5000 0.0000 0.5000 0.01204(12) Uani d S 1
Br Br1 0.41777(7) 0.17716(7) 0.56344(5) 0.01620(17) Uani d . 1
Br Br2 0.23487(7) -0.18757(7) 0.42280(6) 0.01797(17) Uani d . 1
Br Br3 0.51341(7) 0.08706(7) 0.31040(5) 0.01729(17) Uani d . 1
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'
As As 0.0499 2.0058 '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'
Re Re -1.0185 7.2310 '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_1
_geom_angle_site_symmetry_3
_geom_angle
C19 As1 C13 . . 111.1(3)
C19 As1 C1 . . 108.0(3)
C13 As1 C1 . . 108.3(3)
C19 As1 C7 . . 113.8(3)
C13 As1 C7 . . 108.7(3)
C1 As1 C7 . . 106.6(3)
C6 C1 C2 . . 120.9(6)
C6 C1 As1 . . 119.7(5)
C2 C1 As1 . . 119.4(5)
C3 C2 C1 . . 118.3(6)
C3 C2 H2 . . 120.8
C1 C2 H2 . . 120.8
C4 C3 C2 . . 120.9(6)
C4 C3 H3 . . 119.6
C2 C3 H3 . . 119.6
C3 C4 C5 . . 120.6(6)
C3 C4 H4 . . 119.7
C5 C4 H4 . . 119.7
C4 C5 C6 . . 119.5(6)
C4 C5 H5 . . 120.2
C6 C5 H5 . . 120.2
C1 C6 C5 . . 119.7(6)
C1 C6 H6 . . 120.2
C5 C6 H6 . . 120.2
C8 C7 C12 . . 120.4(6)
C8 C7 As1 . . 118.6(5)
C12 C7 As1 . . 120.8(5)
C7 C8 C9 . . 120.0(6)
C7 C8 H8 . . 120.0
C9 C8 H8 . . 120.0
C8 C9 C10 . . 120.3(6)
C8 C9 H9 . . 119.9
C10 C9 H9 . . 119.9
C11 C10 C9 . . 119.2(6)
C11 C10 H10 . . 120.4
C9 C10 H10 . . 120.4
C12 C11 C10 . . 120.1(6)
C12 C11 H11 . . 120.0
C10 C11 H11 . . 120.0
C11 C12 C7 . . 120.1(7)
C11 C12 H12 . . 119.9
C7 C12 H12 . . 119.9
C14 C13 C18 . . 120.2(6)
C14 C13 As1 . . 120.8(5)
C18 C13 As1 . . 119.1(5)
C13 C14 C15 . . 120.4(6)
C13 C14 H14 . . 119.8
C15 C14 H14 . . 119.8
C14 C15 C16 . . 118.9(6)
C14 C15 H15 . . 120.6
C16 C15 H15 . . 120.6
C17 C16 C15 . . 121.2(6)
C17 C16 H16 . . 119.4
C15 C16 H16 . . 119.4
C16 C17 C18 . . 119.9(6)
C16 C17 H17 . . 120.1
C18 C17 H17 . . 120.1
C17 C18 C13 . . 119.3(6)
C17 C18 H18 . . 120.3
C13 C18 H18 . . 120.3
C24 C19 C20 . . 120.9(6)
C24 C19 As1 . . 119.2(5)
C20 C19 As1 . . 119.6(5)
C21 C20 C19 . . 119.0(7)
C21 C20 H20 . . 120.5
C19 C20 H20 . . 120.5
C22 C21 C20 . . 120.2(7)
C22 C21 H21 . . 119.9
C20 C21 H21 . . 119.9
C23 C22 C21 . . 119.8(7)
C23 C22 H22 . . 120.1
C21 C22 H22 . . 120.1
C22 C23 C24 . . 120.6(7)
C22 C23 H23 . . 119.7
C24 C23 H23 . . 119.7
C19 C24 C23 . . 119.5(6)
C19 C24 H24 . . 120.3
C23 C24 H24 . . 120.3
Br1 Re1 Br1 . 2_656 180.0
Br1 Re1 Br3 . 2_656 88.25(2)
Br1 Re1 Br3 2_656 2_656 91.75(2)
Br1 Re1 Br3 . . 91.75(2)
Br1 Re1 Br3 2_656 . 88.25(2)
Br3 Re1 Br3 2_656 . 180.0
Br1 Re1 Br2 . 2_656 89.56(2)
Br1 Re1 Br2 2_656 2_656 90.44(2)
Br3 Re1 Br2 2_656 2_656 89.75(2)
Br3 Re1 Br2 . 2_656 90.25(2)
Br1 Re1 Br2 . . 90.44(2)
Br1 Re1 Br2 2_656 . 89.56(2)
Br3 Re1 Br2 2_656 . 90.25(2)
Br3 Re1 Br2 . . 89.74(2)
Br2 Re1 Br2 2_656 . 180.0
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
As1 C19 . 1.910(6) ?
As1 C13 . 1.914(6) ?
As1 C1 . 1.922(6) ?
As1 C7 . 1.924(6) ?
C1 C6 . 1.380(9) ?
C1 C2 . 1.405(8) ?
C2 C3 . 1.386(9) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.371(9) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.387(9) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.389(9) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.375(9) ?
C7 C12 . 1.383(9) ?
C8 C9 . 1.386(9) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.394(9) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.393(9) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.383(9) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C13 C14 . 1.376(9) ?
C13 C18 . 1.406(9) ?
C14 C15 . 1.388(9) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.392(9) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.375(9) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.385(9) ?
C17 H17 . 0.9300 ?
C18 H18 . 0.9300 ?
C19 C24 . 1.365(9) ?
C19 C20 . 1.391(9) ?
C20 C21 . 1.386(9) ?
C20 H20 . 0.9300 ?
C21 C22 . 1.385(10) ?
C21 H21 . 0.9300 ?
C22 C23 . 1.370(10) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.388(9) ?
C23 H23 . 0.9300 ?
C24 H24 . 0.9300 ?
Re1 Br1 . 2.5023(7) y
Re1 Br1 2_656 2.5023(7) ?
Re1 Br3 2_656 2.5197(7) ?
Re1 Br3 . 2.5197(7) y
Re1 Br2 2_656 2.5264(7) ?
Re1 Br2 . 2.5264(7) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C20 H20 Br1 0.93 2.86 3.671(6) 147
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C19 As1 C1 C6 177.1(5)
C13 As1 C1 C6 -62.5(6)
C7 As1 C1 C6 54.4(6)
C19 As1 C1 C2 -3.0(6)
C13 As1 C1 C2 117.4(5)
C7 As1 C1 C2 -125.7(5)
C6 C1 C2 C3 2.0(10)
As1 C1 C2 C3 -177.9(5)
C1 C2 C3 C4 0.0(10)
C2 C3 C4 C5 -2.4(11)
C3 C4 C5 C6 2.9(10)
C2 C1 C6 C5 -1.5(10)
As1 C1 C6 C5 178.4(5)
C4 C5 C6 C1 -0.9(10)
C19 As1 C7 C8 -70.8(5)
C13 As1 C7 C8 164.7(5)
C1 As1 C7 C8 48.2(5)
C19 As1 C7 C12 113.8(5)
C13 As1 C7 C12 -10.6(6)
C1 As1 C7 C12 -127.2(5)
C12 C7 C8 C9 0.4(9)
As1 C7 C8 C9 -175.0(5)
C7 C8 C9 C10 1.2(10)
C8 C9 C10 C11 -1.8(9)
C9 C10 C11 C12 0.8(9)
C10 C11 C12 C7 0.8(9)
C8 C7 C12 C11 -1.4(9)
As1 C7 C12 C11 173.9(5)
C19 As1 C13 C14 124.9(5)
C1 As1 C13 C14 6.4(6)
C7 As1 C13 C14 -109.1(5)
C19 As1 C13 C18 -56.6(6)
C1 As1 C13 C18 -175.1(5)
C7 As1 C13 C18 69.5(5)
C18 C13 C14 C15 -2.7(9)
As1 C13 C14 C15 175.9(5)
C13 C14 C15 C16 0.7(9)
C14 C15 C16 C17 0.8(10)
C15 C16 C17 C18 -0.2(10)
C16 C17 C18 C13 -1.8(10)
C14 C13 C18 C17 3.2(9)
As1 C13 C18 C17 -175.3(5)
C13 As1 C19 C24 -38.6(6)
C1 As1 C19 C24 80.1(6)
C7 As1 C19 C24 -161.7(5)
C13 As1 C19 C20 148.1(5)
C1 As1 C19 C20 -93.3(5)
C7 As1 C19 C20 24.9(6)
C24 C19 C20 C21 -2.2(10)
As1 C19 C20 C21 171.1(5)
C19 C20 C21 C22 1.6(10)
C20 C21 C22 C23 0.3(11)
C21 C22 C23 C24 -1.7(11)
C20 C19 C24 C23 0.8(10)
As1 C19 C24 C23 -172.4(5)
