#------------------------------------------------------------------------------
#$Date: 2015-06-05 03:21:17 +0300 (Fri, 05 Jun 2015) $
#$Revision: 138060 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/30/4513007.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_4513007
loop_
_publ_author_name
'Martínez-Lillo, José'
'Pedersen, Anders H.'
'Faus, Juan'
'Julve, Miguel'
'Brechin, Euan K.'
_publ_section_title
;
 Effect of Protonated Organic Cations and Anion−π Interactions on
 the Magnetic Behavior of Hexabromorhenate(IV) Salts
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2598
_journal_paper_doi               10.1021/acs.cgd.5b00436
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         '2(C8 H7 N4), Br6 Re, 4(H2 O)'
_chemical_formula_sum            'C16 H22 Br6 N8 O4 Re'
_chemical_formula_weight         1056.08
_chemical_name_systematic
; 
 ? 
;
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.521(3)
_cell_angle_beta                 92.258(2)
_cell_angle_gamma                101.047(2)
_cell_formula_units_Z            2
_cell_length_a                   7.00853(19)
_cell_length_b                   14.2899(4)
_cell_length_c                   14.7561(5)
_cell_measurement_temperature    120(2)
_cell_volume                     1358.51(8)
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_molecular_graphics    'DIAMOND 3.2d (Crystal Impact, 2000)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52753
_diffrn_reflns_theta_full        32.93
_diffrn_reflns_theta_max         32.93
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    13.336
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             982
_exptl_crystal_size_max          0.4518
_exptl_crystal_size_mid          0.1922
_exptl_crystal_size_min          0.1394
_refine_diff_density_max         1.325
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.00139(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         9605
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0291
_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)+(0.0196P)²+0.2837P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0555
_reflns_number_gt                8307
_reflns_number_total             9605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00436_si_002.cif
_cod_data_source_block           eb4062
_cod_depositor_comments
'Adding full bibliography for 4513007--4513008.cif.'
_cod_original_cell_volume        1358.52(7)
_cod_database_code               4513007
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Re1 Re 0.0000 0.0000 0.0000 0.00891(4) Uani 1 2 d S
Re2 Re 0.0000 0.5000 0.5000 0.00906(4) Uani 1 2 d S
Br1 Br 0.06227(4) -0.15930(2) -0.122430(19) 0.01378(6) Uani 1 1 d .
Br2 Br -0.15732(4) -0.10054(2) 0.098567(19) 0.01252(6) Uani 1 1 d .
Br3 Br -0.32638(4) -0.02814(2) -0.093938(19) 0.01266(6) Uani 1 1 d .
Br4 Br 0.10386(4) 0.39627(2) 0.59307(2) 0.01382(6) Uani 1 1 d .
Br5 Br -0.29054(4) 0.51782(2) 0.59483(2) 0.01510(6) Uani 1 1 d .
Br6 Br 0.19579(5) 0.65803(2) 0.62777(2) 0.01632(7) Uani 1 1 d .
N1 N 0.3672(4) 0.08584(19) 0.61844(17) 0.0146(5) Uani 1 1 d .
N2 N 0.2090(4) -0.07097(19) 0.49518(17) 0.0140(5) Uani 1 1 d .
N3 N 0.1659(4) 0.03825(19) 0.37562(17) 0.0138(5) Uani 1 1 d .
N4 N 0.3525(4) 0.1849(2) 0.49421(17) 0.0136(5) Uani 1 1 d .
H4A H 0.425(5) 0.218(3) 0.549(3) 0.022(10) Uiso 1 1 d .
N5 N 0.7940(4) 0.41866(19) -0.10677(17) 0.0139(5) Uani 1 1 d .
N6 N 0.7666(4) 0.57493(19) 0.01480(17) 0.0144(5) Uani 1 1 d .
N7 N 0.6272(4) 0.4660(2) 0.12876(17) 0.0146(5) Uani 1 1 d .
N8 N 0.6361(4) 0.3138(2) 0.00388(18) 0.0120(5) Uani 1 1 d .
H8A H 0.661(8) 0.283(4) -0.049(4) 0.09(2) Uiso 1 1 d .
O1W O 0.7215(4) 0.70837(19) 0.22107(17) 0.0268(5) Uani 1 1 d D
H1WA H 0.706(6) 0.6449(17) 0.170(2) 0.057(14) Uiso 1 1 d D
H1WB H 0.619(5) 0.700(3) 0.260(3) 0.058(15) Uiso 1 1 d D
O2W O 0.2742(3) 0.81587(17) 0.14923(15) 0.0179(5) Uani 1 1 d D
H2WA H 0.190(5) 0.796(3) 0.192(3) 0.058(14) Uiso 1 1 d D
H2WB H 0.218(6) 0.868(2) 0.140(3) 0.051(14) Uiso 1 1 d D
O3W O 0.1025(3) 0.78199(17) 0.29864(15) 0.0191(5) Uani 1 1 d D
H3WA H -0.032(2) 0.751(3) 0.281(3) 0.061(15) Uiso 1 1 d D
H3WB H 0.113(6) 0.8455(18) 0.349(2) 0.065(15) Uiso 1 1 d D
O4W O 0.3976(3) 0.69560(17) 0.34901(16) 0.0193(5) Uani 1 1 d D
H4WA H 0.297(5) 0.721(3) 0.325(3) 0.074(17) Uiso 1 1 d D
H4WB H 0.325(5) 0.638(2) 0.359(3) 0.054(14) Uiso 1 1 d D
C1 C 0.2815(4) 0.0293(2) 0.5299(2) 0.0121(6) Uani 1 1 d .
C2 C 0.3800(5) 0.0358(2) 0.6802(2) 0.0167(6) Uani 1 1 d .
H2B H 0.4372 0.0721 0.7433 0.020 Uiso 1 1 calc R
C3 C 0.3110(5) -0.0680(2) 0.6530(2) 0.0157(6) Uani 1 1 d .
H3B H 0.3203 -0.1020 0.6962 0.019 Uiso 1 1 calc R
C4 C 0.2270(5) -0.1194(2) 0.5580(2) 0.0159(6) Uani 1 1 d .
H4B H 0.1817 -0.1895 0.5372 0.019 Uiso 1 1 calc R
C5 C 0.2647(4) 0.0855(2) 0.4626(2) 0.0117(5) Uani 1 1 d .
C6 C 0.1529(4) 0.0947(2) 0.3196(2) 0.0152(6) Uani 1 1 d .
H6B H 0.0839 0.0632 0.2583 0.018 Uiso 1 1 calc R
C7 C 0.2373(5) 0.1977(2) 0.3489(2) 0.0166(6) Uani 1 1 d .
H7B H 0.2245 0.2350 0.3089 0.020 Uiso 1 1 calc R
C8 C 0.3411(4) 0.2427(2) 0.4397(2) 0.0133(6) Uani 1 1 d .
H8B H 0.4015 0.3114 0.4625 0.016 Uiso 1 1 calc R
C9 C 0.7446(4) 0.4740(2) -0.02202(19) 0.0109(5) Uani 1 1 d .
C10 C 0.8763(4) 0.4720(2) -0.1598(2) 0.0136(6) Uani 1 1 d .
H10A H 0.9161 0.4373 -0.2187 0.016 Uiso 1 1 calc R
C11 C 0.9042(4) 0.5764(2) -0.1302(2) 0.0151(6) Uani 1 1 d .
H11A H 0.9584 0.6122 -0.1687 0.018 Uiso 1 1 calc R
C12 C 0.8482(4) 0.6259(2) -0.0405(2) 0.0157(6) Uani 1 1 d .
H12A H 0.8678 0.6964 -0.0182 0.019 Uiso 1 1 calc R
C13 C 0.6629(4) 0.4161(2) 0.04006(19) 0.0111(5) Uani 1 1 d .
C14 C 0.5617(5) 0.4096(3) 0.1824(2) 0.0180(6) Uani 1 1 d .
H14A H 0.5377 0.4428 0.2454 0.022 Uiso 1 1 calc R
C15 C 0.5280(5) 0.3047(3) 0.1488(2) 0.0173(6) Uani 1 1 d .
H15A H 0.4800 0.2677 0.1875 0.021 Uiso 1 1 calc R
C16 C 0.5680(4) 0.2567(2) 0.0564(2) 0.0146(6) Uani 1 1 d .
H16A H 0.5482 0.1862 0.0308 0.018 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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Br2 Re1 Br2 180.000(10) . 2
Br2 Re1 Br1 90.576(9) . .
Br2 Re1 Br1 89.424(9) 2 .
Br2 Re1 Br1 89.424(9) . 2
Br2 Re1 Br1 90.576(9) 2 2
Br1 Re1 Br1 180.000(19) . 2
Br2 Re1 Br3 90.273(9) . .
Br2 Re1 Br3 89.727(9) 2 .
Br1 Re1 Br3 89.809(10) . .
Br1 Re1 Br3 90.191(10) 2 .
Br2 Re1 Br3 89.727(9) . 2
Br2 Re1 Br3 90.273(9) 2 2
Br1 Re1 Br3 90.191(10) . 2
Br1 Re1 Br3 89.809(10) 2 2
Br3 Re1 Br3 180.000(14) . 2
Br6 Re2 Br6 180.0 2_566 .
Br6 Re2 Br4 90.771(10) 2_566 .
Br6 Re2 Br4 89.229(10) . .
Br6 Re2 Br4 89.229(10) 2_566 2_566
Br6 Re2 Br4 90.771(10) . 2_566
Br4 Re2 Br4 180.000(9) . 2_566
Br6 Re2 Br5 90.839(11) 2_566 .
Br6 Re2 Br5 89.161(10) . .
Br4 Re2 Br5 89.143(10) . .
Br4 Re2 Br5 90.857(10) 2_566 .
Br6 Re2 Br5 89.161(10) 2_566 2_566
Br6 Re2 Br5 90.839(11) . 2_566
Br4 Re2 Br5 90.857(9) . 2_566
Br4 Re2 Br5 89.143(9) 2_566 2_566
Br5 Re2 Br5 180.0 . 2_566
C1 N1 C2 115.7(3) . .
C1 N2 C4 115.2(3) . .
C5 N3 C6 116.9(3) . .
C8 N4 C5 121.6(3) . .
C8 N4 H4A 113(2) . .
C5 N4 H4A 126(2) . .
C9 N5 C10 115.2(3) . .
C9 N6 C12 115.4(2) . .
C13 N7 C14 116.6(3) . .
C16 N8 C13 121.1(3) . .
C16 N8 H8A 115(4) . .
C13 N8 H8A 124(4) . .
H1WA O1W H1WB 106(3) . .
H2WA O2W H2WB 101(2) . .
H3WA O3W H3WB 108(3) . .
H4WA O4W H4WB 102(3) . .
N1 C1 N2 127.8(3) . .
N1 C1 C5 115.4(3) . .
N2 C1 C5 116.8(3) . .
N1 C2 C3 122.0(3) . .
N1 C2 H2B 119.0 . .
C3 C2 H2B 119.0 . .
C2 C3 C4 117.1(3) . .
C2 C3 H3B 121.5 . .
C4 C3 H3B 121.5 . .
N2 C4 C3 122.2(3) . .
N2 C4 H4B 118.9 . .
C3 C4 H4B 118.9 . .
N3 C5 N4 122.5(3) . .
N3 C5 C1 120.3(3) . .
N4 C5 C1 117.2(3) . .
N3 C6 C7 123.2(3) . .
N3 C6 H6B 118.4 . .
C7 C6 H6B 118.4 . .
C8 C7 C6 117.5(3) . .
C8 C7 H7B 121.3 . .
C6 C7 H7B 121.3 . .
N4 C8 C7 118.3(3) . .
N4 C8 H8B 120.8 . .
C7 C8 H8B 120.8 . .
N6 C9 N5 127.8(3) . .
N6 C9 C13 116.4(2) . .
N5 C9 C13 115.8(2) . .
N5 C10 C11 122.5(3) . .
N5 C10 H10A 118.8 . .
C11 C10 H10A 118.8 . .
C10 C11 C12 117.2(3) . .
C10 C11 H11A 121.4 . .
C12 C11 H11A 121.4 . .
N6 C12 C11 121.9(3) . .
N6 C12 H12A 119.0 . .
C11 C12 H12A 119.0 . .
N7 C13 N8 122.8(3) . .
N7 C13 C9 119.5(3) . .
N8 C13 C9 117.6(2) . .
N7 C14 C15 123.3(3) . .
N7 C14 H14A 118.4 . .
C15 C14 H14A 118.4 . .
C16 C15 C14 117.7(3) . .
C16 C15 H15A 121.1 . .
C14 C15 H15A 121.1 . .
N8 C16 C15 118.5(3) . .
N8 C16 H16A 120.8 . .
C15 C16 H16A 120.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 Br2 2.5122(3) .
Re1 Br2 2.5122(3) 2
Re1 Br1 2.5161(3) .
Re1 Br1 2.5161(3) 2
Re1 Br3 2.5181(3) .
Re1 Br3 2.5181(3) 2
Re2 Br6 2.5101(3) 2_566
Re2 Br6 2.5101(3) .
Re2 Br4 2.5117(3) .
Re2 Br4 2.5117(3) 2_566
Re2 Br5 2.5208(3) .
Re2 Br5 2.5208(3) 2_566
N1 C1 1.329(4) .
N1 C2 1.344(4) .
N2 C1 1.335(4) .
N2 C4 1.344(4) .
N3 C5 1.324(4) .
N3 C6 1.346(4) .
N4 C8 1.341(4) .
N4 C5 1.347(4) .
N4 H4A 0.87(4) .
N5 C9 1.337(4) .
N5 C10 1.338(4) .
N6 C9 1.335(4) .
N6 C12 1.341(4) .
N7 C13 1.325(3) .
N7 C14 1.342(4) .
N8 C16 1.340(4) .
N8 C13 1.349(4) .
N8 H8A 0.80(5) .
O1W H1WA 0.946(10) .
O1W H1WB 0.950(10) .
O2W H2WA 0.951(10) .
O2W H2WB 0.953(10) .
O3W H3WA 0.950(10) .
O3W H3WB 0.947(10) .
O4W H4WA 0.954(10) .
O4W H4WB 0.944(10) .
C1 C5 1.486(4) .
C2 C3 1.380(4) .
C2 H2B 0.9300 .
C3 C4 1.390(4) .
C3 H3B 0.9300 .
C4 H4B 0.9300 .
C6 C7 1.386(4) .
C6 H6B 0.9300 .
C7 C8 1.381(4) .
C7 H7B 0.9300 .
C8 H8B 0.9300 .
C9 C13 1.490(4) .
C10 C11 1.379(4) .
C10 H10A 0.9300 .
C11 C12 1.388(4) .
C11 H11A 0.9300 .
C12 H12A 0.9300 .
C14 C15 1.381(5) .
C14 H14A 0.9300 .
C15 C16 1.374(4) .
C15 H15A 0.9300 .
C16 H16A 0.9300 .
