#------------------------------------------------------------------------------
#$Date: 2015-06-05 03:21:17 +0300 (Fri, 05 Jun 2015) $
#$Revision: 138060 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/30/4513008.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_4513008
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         'C6 H8 N4, Br6 Re, 4(H2 O)'
_chemical_formula_sum            'C6 H16 Br6 N4 O4 Re'
_chemical_formula_weight         873.89
_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                108.544(5)
_cell_angle_beta                 111.239(6)
_cell_angle_gamma                99.162(5)
_cell_formula_units_Z            1
_cell_length_a                   8.2613(5)
_cell_length_b                   8.3131(5)
_cell_length_c                   8.3431(5)
_cell_measurement_reflns_used    5223
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      29.3180
_cell_measurement_theta_min      3.8010
_cell_volume                     481.30(6)
_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      120.0
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8714
_diffrn_reflns_theta_full        29.74
_diffrn_reflns_theta_max         29.74
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    18.780
_exptl_absorpt_correction_T_max  0.229
_exptl_absorpt_correction_T_min  0.084
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             397
_exptl_crystal_size_max          0.1939
_exptl_crystal_size_mid          0.1565
_exptl_crystal_size_min          0.1001
_refine_diff_density_max         0.712
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2401
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0233
_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)+(0.0232P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0515
_reflns_number_gt                2259
_reflns_number_total             2401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00436_si_003.cif
_cod_data_source_block           eb4120
_cod_depositor_comments
'Adding full bibliography for 4513007--4513008.cif.'
_cod_original_cell_volume        481.29(5)
_cod_database_code               4513008
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 0.5000 0.0000 0.5000 0.00830(7) Uani 1 2 d S
Br1 Br 0.43140(5) -0.32280(4) 0.44493(5) 0.01404(9) Uani 1 1 d .
Br2 Br 0.56213(5) 0.08053(5) 0.83926(5) 0.01499(9) Uani 1 1 d .
Br3 Br 0.82799(5) 0.02186(5) 0.58444(5) 0.01371(9) Uani 1 1 d .
N1 N 0.9641(4) 0.6653(4) 0.8936(4) 0.0140(7) Uani 1 1 d .
H1A H 1.0349 0.6685 0.8396 0.017 Uiso 1 1 calc R
N2 N 0.8288(4) 0.5987(4) 1.0532(4) 0.0145(7) Uani 1 1 d .
H2A H 0.7969 0.5510 1.1191 0.017 Uiso 1 1 calc R
C1 C 0.8456(5) 0.7639(5) 0.8970(5) 0.0167(8) Uani 1 1 d .
H1B H 0.8262 0.8437 0.8406 0.020 Uiso 1 1 calc R
C2 C 0.7629(5) 0.7229(5) 0.9976(6) 0.0171(8) Uani 1 1 d .
H2B H 0.6764 0.7703 1.0245 0.020 Uiso 1 1 calc R
C3 C 0.9517(5) 0.5636(5) 0.9878(5) 0.0126(7) Uani 1 1 d .
O1W O 0.2280(4) 0.4427(4) 0.6586(4) 0.0244(7) Uani 1 1 d D
O2W O 0.8743(4) 0.2583(4) 0.3224(4) 0.0249(7) Uani 1 1 d D
H1WA H 0.332(6) 0.431(8) 0.637(10) 0.10(3) Uiso 1 1 d D
H2WA H 0.964(6) 0.285(8) 0.446(4) 0.09(2) Uiso 1 1 d D
H2WB H 0.777(5) 0.163(6) 0.302(8) 0.07(2) Uiso 1 1 d D
H1WB H 0.226(7) 0.556(4) 0.655(9) 0.063(19) Uiso 1 1 d D
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
Br3 Re1 Br3 180.0 . 2_656
Br3 Re1 Br1 89.538(13) . .
Br3 Re1 Br1 90.462(13) 2_656 .
Br3 Re1 Br1 90.462(13) . 2_656
Br3 Re1 Br1 89.538(13) 2_656 2_656
Br1 Re1 Br1 180.0 . 2_656
Br3 Re1 Br2 90.183(14) . .
Br3 Re1 Br2 89.817(14) 2_656 .
Br1 Re1 Br2 89.349(14) . .
Br1 Re1 Br2 90.651(14) 2_656 .
Br3 Re1 Br2 89.817(14) . 2_656
Br3 Re1 Br2 90.183(14) 2_656 2_656
Br1 Re1 Br2 90.651(14) . 2_656
Br1 Re1 Br2 89.349(14) 2_656 2_656
Br2 Re1 Br2 180.0 . 2_656
C3 N1 C1 109.2(3) . .
C3 N1 H1A 125.4 . .
C1 N1 H1A 125.4 . .
C3 N2 C2 108.8(3) . .
C3 N2 H2A 125.6 . .
C2 N2 H2A 125.6 . .
C2 C1 N1 106.9(3) . .
C2 C1 H1B 126.5 . .
N1 C1 H1B 126.5 . .
C1 C2 N2 107.7(3) . .
C1 C2 H2B 126.1 . .
N2 C2 H2B 126.1 . .
N1 C3 N2 107.3(3) . .
N1 C3 C3 126.9(5) . 2_767
N2 C3 C3 125.7(5) . 2_767
H1WA O1W H1WB 100(3) . .
H2WA O2W H2WB 103(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 Br3 2.5000(4) .
Re1 Br3 2.5000(4) 2_656
Re1 Br1 2.5052(4) .
Re1 Br1 2.5052(4) 2_656
Re1 Br2 2.5211(4) .
Re1 Br2 2.5211(4) 2_656
N1 C3 1.341(5) .
N1 C1 1.376(5) .
N1 H1A 0.8600 .
N2 C3 1.344(5) .
N2 C2 1.371(5) .
N2 H2A 0.8600 .
C1 C2 1.345(6) .
C1 H1B 0.9300 .
C2 H2B 0.9300 .
C3 C3 1.443(7) 2_767
O1W H1WA 0.957(10) .
O1W H1WB 0.957(10) .
O2W H2WA 0.955(10) .
O2W H2WB 0.956(10) .
