#------------------------------------------------------------------------------
#$Date: 2017-11-10 11:32:19 +0200 (Fri, 10 Nov 2017) $
#$Revision: 203046 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/79/1547957.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_1547957
loop_
_publ_author_name
'Christopher H. Woodall'
'Gavin A. Craig'
'Alessandro Prescimone'
'Martin Misek'
'Joan Cano'
'Juan Faus'
'Michael R. Probert'
'Simon Parsons'
'Stephen Moggach'
'Jose Martinez-Lillo'
'Mark Murrie'
'Konstantin V. Kamenev'
'Euan K. Brechin'
_publ_section_title
;
 Pressure induced enhancement of the magnetic ordering temperature in
 rhenium(IV) monomers
;
_journal_name_full               'Nature Communications'
_journal_page_first              13870
_journal_paper_doi               10.1038/ncomms13870
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C8 H6 Br4 N4 Re'
_chemical_formula_sum            'C8 H6 Br4 N4 Re'
_chemical_formula_weight         664.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6184(4)
_cell_length_b                   10.8488(4)
_cell_length_c                   13.4471(4)
_cell_measurement_temperature    293
_cell_volume                     1403.18(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.560
_diffrn_measured_fraction_theta_max 0.523
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'CSEC APEX2 HP'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.560
_diffrn_reflns_Laue_measured_fraction_max 0.523
_diffrn_reflns_number            920
_diffrn_reflns_point_group_measured_fraction_full 0.324
_diffrn_reflns_point_group_measured_fraction_max 0.301
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.981
_diffrn_reflns_theta_min         2.830
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.988
_exptl_absorpt_correction_T_max  0.745468
_exptl_absorpt_correction_T_min  0.454923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0951 before and 0.0542 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1326 before and 0.0578 after correction.
 The Ratio of minimum to maximum transmission is 0.61.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 15036 reflections, Rint = 0.0619
 (10217 with I > 3sig(I), Rint = 0.0528)
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.143
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.721
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.257
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.52(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0369P)²+34.9890P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                830
_reflns_number_total             920
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ReBr4bpymambientincell.cif
_cod_data_source_block           shelxs
_cod_database_code               1547957
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C1(H1), C7(H7), C8(H8)
2.b Fitted hexagon refined as free rotating group:
 N4(C2,N2,C4,C5,C6), C1(N1,C3,N3,C7,C8)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.10862(14) 0.08473(12) 0.11317(7) 0.0361(3) Uani 1 1 d . . . . .
Br1 Br 0.1192(5) 0.3087(3) 0.1274(3) 0.0645(11) Uani 1 1 d . . . . .
Br2 Br 0.3533(4) 0.0674(4) 0.0619(2) 0.0523(10) Uani 1 1 d . . . . .
Br3 Br -0.1481(4) 0.0784(4) 0.1366(2) 0.0577(10) Uani 1 1 d . . . . .
Br4 Br 0.1589(5) 0.0522(4) 0.2889(2) 0.0611(13) Uani 1 1 d . . . . .
N4 N 0.059(3) -0.2501(16) -0.0556(10) 0.054(8) Uiso 1 1 d . . . . .
C2 C 0.056(3) -0.1299(14) -0.0198(11) 0.042(8) Uiso 1 1 d G . . . .
N2 N 0.097(3) -0.1054(13) 0.0773(12) 0.043(6) Uiso 1 1 d G . . . .
C4 C 0.141(3) -0.2011(18) 0.1386(10) 0.065(10) Uiso 1 1 d G . . . .
H4 H 0.1684 -0.1847 0.2036 0.078 Uiso 1 1 calc R . . . .
C5 C 0.143(3) -0.3213(16) 0.1028(13) 0.059(9) Uiso 1 1 d G . . . .
H5 H 0.1722 -0.3853 0.1439 0.071 Uiso 1 1 calc R . . . .
C6 C 0.102(3) -0.3458(13) 0.0057(13) 0.042(7) Uiso 1 1 d G . . . .
H6 H 0.1035 -0.4262 -0.0182 0.050 Uiso 1 1 calc R . . . .
C1 C 0.053(2) 0.1841(14) -0.1035(13) 0.043(8) Uiso 1 1 d . . . . .
H1 H 0.0810 0.2613 -0.0815 0.052 Uiso 1 1 calc R . . . .
N1 N 0.062(2) 0.0828(17) -0.0405(10) 0.032(5) Uiso 1 1 d G . . . .
C3 C 0.019(2) -0.0327(14) -0.0734(11) 0.051(9) Uiso 1 1 d G . . . .
N3 N -0.033(2) -0.0469(13) -0.1691(12) 0.036(6) Uiso 1 1 d G . . . .
C7 C -0.042(2) 0.0544(17) -0.2321(10) 0.054(10) Uiso 1 1 d G . . . .
H7 H -0.0768 0.0449 -0.2961 0.065 Uiso 1 1 calc R . . . .
C8 C 0.001(3) 0.1699(14) -0.1992(13) 0.050(9) Uiso 1 1 d G . . . .
H8 H -0.0058 0.2377 -0.2413 0.060 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 0.0030 0.0020 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 '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
Br1 Re1 Br2 93.33(15) . .
Br1 Re1 Br3 93.37(16) . .
Br2 Re1 Br3 169.17(12) . .
Br4 Re1 Br1 93.42(14) . .
Br4 Re1 Br2 94.05(14) . .
Br4 Re1 Br3 94.04(14) . .
N2 Re1 Br1 171.3(5) . .
N2 Re1 Br2 84.9(7) . .
N2 Re1 Br3 87.2(7) . .
N2 Re1 Br4 95.2(5) . .
N1 Re1 Br1 95.5(5) . .
N1 Re1 Br2 85.9(5) . .
N1 Re1 Br3 85.0(5) . .
N1 Re1 Br4 171.1(5) . .
N1 Re1 N2 75.9(7) . .
C2 N4 C6 120.0 . .
N4 C2 N2 120.0 . .
C3 C2 N4 124.2(14) . .
C3 C2 N2 115.8(14) . .
C2 N2 Re1 114.5(9) . .
C4 N2 Re1 125.2(9) . .
C4 N2 C2 120.0 . .
N2 C4 H4 120.0 . .
C5 C4 N2 120.0 . .
C5 C4 H4 120.0 . .
C4 C5 H5 120.0 . .
C4 C5 C6 120.0 . .
C6 C5 H5 120.0 . .
N4 C6 H6 120.0 . .
C5 C6 N4 120.0 . .
C5 C6 H6 120.0 . .
N1 C1 H1 120.0 . .
N1 C1 C8 120.0 . .
C8 C1 H1 120.0 . .
C1 N1 Re1 126.9(10) . .
C1 N1 C3 120.0 . .
C3 N1 Re1 112.5(9) . .
C2 C3 N1 117.7(15) . .
C2 C3 N3 120.8(14) . .
N1 C3 N3 120.0 . .
C7 N3 C3 120.0 . .
N3 C7 H7 120.0 . .
N3 C7 C8 120.0 . .
C8 C7 H7 120.0 . .
C1 C8 H8 120.0 . .
C7 C8 C1 120.0 . .
C7 C8 H8 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 Br1 2.439(4) .
Re1 Br2 2.460(4) .
Re1 Br3 2.490(4) .
Re1 Br4 2.438(3) .
Re1 N2 2.121(14) .
Re1 N1 2.115(12) .
N4 C2 1.3900 .
N4 C6 1.3900 .
C2 N2 1.3900 .
C2 C3 1.325(18) .
N2 C4 1.3900 .
C4 H4 0.9300 .
C4 C5 1.3900 .
C5 H5 0.9300 .
C5 C6 1.3900 .
C6 H6 0.9300 .
C1 H1 0.9300 .
C1 N1 1.3900 .
C1 C8 1.3900 .
N1 C3 1.3900 .
C3 N3 1.3900 .
N3 C7 1.3900 .
C7 H7 0.9300 .
C7 C8 1.3900 .
C8 H8 0.9300 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Re1 N2 C4 C5 -172.7(16) . . . .
Re1 N1 C3 C2 -22.1(18) . . . .
Re1 N1 C3 N3 171.6(13) . . . .
N4 C2 N2 Re1 173.4(15) . . . .
N4 C2 N2 C4 0.0 . . . .
N4 C2 C3 N1 -160.3(13) . . . .
N4 C2 C3 N3 6(3) . . . .
C2 N4 C6 C5 0.0 . . . .
C2 N2 C4 C5 0.0 . . . .
C2 C3 N3 C7 -166(2) . . . .
N2 C2 C3 N1 18(2) . . . .
N2 C2 C3 N3 -175.6(12) . . . .
N2 C4 C5 C6 0.0 . . . .
C4 C5 C6 N4 0.0 . . . .
C6 N4 C2 N2 0.0 . . . .
C6 N4 C2 C3 179(3) . . . .
C1 N1 C3 C2 166(2) . . . .
C1 N1 C3 N3 0.0 . . . .
N1 C1 C8 C7 0.0 . . . .
N1 C3 N3 C7 0.0 . . . .
C3 C2 N2 Re1 -5(2) . . . .
C3 C2 N2 C4 -179(2) . . . .
C3 N3 C7 C8 0.0 . . . .
N3 C7 C8 C1 0.0 . . . .
C8 C1 N1 Re1 -170.3(15) . . . .
C8 C1 N1 C3 0.0 . . . .
