#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:36:26 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180147 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/44/7104488.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_7104488
loop_
_publ_author_name
'Nieto, Sonia'
'Pérez, Julio'
'Riera, Lucía'
'Riera, Víctor'
'Miguel, Daniel'
_publ_section_title
;
 Metal complexes with two different hydrogen-bond donor ligands as
 anion hosts.
;
_journal_issue                   22
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3279
_journal_page_last               3281
_journal_paper_doi               10.1039/b823460d
_journal_volume                  34
_journal_year                    2009
_chemical_formula_sum            'C18 H23 Br N6 O4 Re'
_chemical_formula_weight         653.53
_chemical_name_systematic
;
?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.396(4)
_cell_angle_beta                 90.268(3)
_cell_angle_gamma                107.713(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3635(3)
_cell_length_b                   8.9590(4)
_cell_length_c                   16.4246(7)
_cell_measurement_reflns_used    7713
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.6103
_cell_measurement_theta_min      5.3530
_cell_volume                     1131.21(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10083
_diffrn_reflns_theta_full        73.89
_diffrn_reflns_theta_max         73.89
_diffrn_reflns_theta_min         5.36
_exptl_absorpt_coefficient_mu    12.887
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.721
_refine_diff_density_min         -2.345
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4179
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0455
_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)+(0.0791P)²+7.5458P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                3822
_reflns_number_total             4179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b823460d.txt
_cod_data_source_block           Compound_2Br_(lr297)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7104488
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.91517(4) 0.74271(4) 0.65536(2) 0.03245(15) Uani 1 1 d . . .
C2 C 0.8350(11) 0.5407(11) 0.5692(6) 0.0408(19) Uani 1 1 d . . .
N3 N 0.6988(8) 0.8252(8) 0.6345(4) 0.0336(14) Uani 1 1 d . . .
N1 N 1.0012(9) 0.9703(8) 0.7578(4) 0.0367(14) Uani 1 1 d . . .
N5 N 0.7596(8) 0.6239(7) 0.7459(4) 0.0335(14) Uani 1 1 d . . .
O1 O 1.1130(8) 0.8989(8) 0.5245(4) 0.0458(14) Uani 1 1 d . . .
O3 O 1.2176(8) 0.6226(8) 0.6856(4) 0.0488(15) Uani 1 1 d . . .
N4 N 0.6388(9) 0.9135(8) 0.6992(4) 0.0379(15) Uani 1 1 d D . .
O2 O 0.7936(9) 0.4202(8) 0.5191(5) 0.0582(18) Uani 1 1 d . . .
N2 N 1.0642(10) 0.9729(9) 0.8346(4) 0.0425(16) Uani 1 1 d . . .
H2 H 1.0658 0.8875 0.8490 0.051 Uiso 1 1 calc R . .
C35 C 0.8352(11) 0.5827(10) 0.8052(5) 0.0367(17) Uani 1 1 d . . .
H331 H 0.9519 0.6093 0.8087 0.044 Uiso 1 1 calc R . .
C31 C 0.5940(11) 0.5821(10) 0.7400(5) 0.0409(19) Uani 1 1 d . . .
H35 H 0.5401 0.6064 0.6978 0.049 Uiso 1 1 calc R . .
C3 C 1.1064(13) 0.6710(10) 0.6752(5) 0.047(2) Uani 1 1 d . . .
C34 C 0.7477(13) 0.5019(10) 0.8621(6) 0.046(2) Uani 1 1 d . . .
C13 C 1.1239(12) 1.1245(11) 0.8856(5) 0.045(2) Uani 1 1 d . . .
C23 C 0.6151(10) 0.8164(10) 0.5646(5) 0.0364(17) Uani 1 1 d . . .
C32 C 0.4966(13) 0.5034(11) 0.7941(6) 0.048(2) Uani 1 1 d . . .
H34 H 0.3799 0.4771 0.7884 0.057 Uiso 1 1 calc R . .
C12 C 1.1010(11) 1.2282(11) 0.8411(6) 0.045(2) Uani 1 1 d . . .
H22 H 1.1296 1.3406 0.8596 0.054 Uiso 1 1 calc R . .
C21 C 0.5159(10) 0.9606(10) 0.6702(6) 0.0407(18) Uani 1 1 d . . .
C1 C 1.0380(10) 0.8427(10) 0.5749(6) 0.0388(18) Uani 1 1 d . . .
C22 C 0.5004(11) 0.9012(10) 0.5857(6) 0.0420(19) Uani 1 1 d . . .
H12 H 0.4258 0.9146 0.5481 0.050 Uiso 1 1 calc R . .
C11 C 1.0243(12) 1.1277(11) 0.7609(6) 0.045(2) Uani 1 1 d . . .
C33 C 0.5730(12) 0.4651(10) 0.8556(6) 0.0423(19) Uani 1 1 d . . .
H33 H 0.5091 0.4147 0.8932 0.051 Uiso 1 1 calc R . .
N6 N 0.8348(12) 0.4677(12) 0.9216(6) 0.062(2) Uani 1 1 d . . .
H32A H 0.7817 0.4208 0.9578 0.075 Uiso 1 1 calc R . .
H32B H 0.9427 0.4929 0.9229 0.075 Uiso 1 1 calc R . .
C25 C 0.6403(12) 0.7269(11) 0.4785(5) 0.046(2) Uani 1 1 d . . .
H14A H 0.7287 0.6806 0.4824 0.070 Uiso 1 1 calc R . .
H14B H 0.6707 0.8006 0.4434 0.070 Uiso 1 1 calc R . .
H14C H 0.5378 0.6419 0.4544 0.070 Uiso 1 1 calc R . .
C14 C 0.9783(14) 1.1851(12) 0.6898(7) 0.056(2) Uani 1 1 d . . .
H24A H 0.9282 1.0937 0.6425 0.083 Uiso 1 1 calc R . .
H24B H 1.0776 1.2560 0.6741 0.083 Uiso 1 1 calc R . .
H24C H 0.8993 1.2430 0.7067 0.083 Uiso 1 1 calc R . .
C24 C 0.4280(12) 1.0597(13) 0.7279(7) 0.052(2) Uani 1 1 d . . .
H15A H 0.4721 1.0804 0.7851 0.079 Uiso 1 1 calc R . .
H15B H 0.3095 1.0017 0.7221 0.079 Uiso 1 1 calc R . .
H15C H 0.4456 1.1609 0.7137 0.079 Uiso 1 1 calc R . .
C15 C 1.2036(18) 1.1571(14) 0.9713(7) 0.068(3) Uani 1 1 d . . .
H25A H 1.1981 1.0562 0.9834 0.102 Uiso 1 1 calc R . .
H25B H 1.1452 1.2137 1.0117 0.102 Uiso 1 1 calc R . .
H25C H 1.3193 1.2226 0.9747 0.102 Uiso 1 1 calc R . .
O10 O 0.6413(12) 0.9657(13) 0.8748(5) 0.067(2) Uani 1 1 d . . .
Br1 Br 0.74617(13) 0.25418(12) 0.07218(6) 0.0485(2) Uani 1 1 d . . .
H112 H 0.673(9) 0.927(9) 0.752(2) 0.017(17) Uiso 1 1 d D . .
H100 H 0.66(2) 1.00(2) 0.909(10) 0.08(6) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 '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
_geom_angle_publ_flag
C1 Re1 C2 89.5(4) . . ?
C1 Re1 C3 88.0(3) . . ?
C2 Re1 C3 85.2(4) . . ?
C1 Re1 N3 92.4(3) . . ?
C2 Re1 N3 95.3(3) . . ?
C3 Re1 N3 179.3(3) . . ?
C1 Re1 N1 92.7(3) . . ?
C2 Re1 N1 177.8(3) . . ?
C3 Re1 N1 95.0(3) . . ?
N3 Re1 N1 84.5(3) . . ?
C1 Re1 N5 177.2(3) . . ?
C2 Re1 N5 89.3(3) . . ?
C3 Re1 N5 94.4(3) . . ?
N3 Re1 N5 85.2(2) . . ?
N1 Re1 N5 88.5(2) . . ?
O2 C2 Re1 177.1(8) . . ?
C23 N3 N4 107.2(7) . . ?
C23 N3 Re1 131.2(6) . . ?
N4 N3 Re1 121.4(5) . . ?
C11 N1 N2 104.9(7) . . ?
C11 N1 Re1 133.4(6) . . ?
N2 N1 Re1 121.3(5) . . ?
C31 N5 C35 117.9(7) . . ?
C31 N5 Re1 122.5(6) . . ?
C35 N5 Re1 119.4(5) . . ?
C21 N4 N3 110.5(7) . . ?
C21 N4 H112 128(5) . . ?
N3 N4 H112 122(5) . . ?
C13 N2 N1 112.4(8) . . ?
C13 N2 H2 123.8 . . ?
N1 N2 H2 123.8 . . ?
N5 C35 C34 123.5(8) . . ?
N5 C35 H331 118.3 . . ?
C34 C35 H331 118.3 . . ?
N5 C31 C32 122.8(9) . . ?
N5 C31 H35 118.6 . . ?
C32 C31 H35 118.6 . . ?
O3 C3 Re1 177.7(7) . . ?
N6 C34 C33 123.6(8) . . ?
N6 C34 C35 119.6(9) . . ?
C33 C34 C35 116.8(9) . . ?
N2 C13 C12 107.2(8) . . ?
N2 C13 C15 121.8(9) . . ?
C12 C13 C15 130.9(9) . . ?
N3 C23 C22 108.3(8) . . ?
N3 C23 C25 124.5(8) . . ?
C22 C23 C25 127.2(8) . . ?
C33 C32 C31 119.4(9) . . ?
C33 C32 H34 120.3 . . ?
C31 C32 H34 120.3 . . ?
C13 C12 C11 105.4(8) . . ?
C13 C12 H22 127.3 . . ?
C11 C12 H22 127.3 . . ?
C22 C21 N4 105.8(7) . . ?
C22 C21 C24 132.3(9) . . ?
N4 C21 C24 121.9(8) . . ?
O1 C1 Re1 177.9(7) . . ?
C21 C22 C23 108.2(8) . . ?
C21 C22 H12 125.9 . . ?
C23 C22 H12 125.9 . . ?
N1 C11 C12 110.1(8) . . ?
N1 C11 C14 124.4(8) . . ?
C12 C11 C14 125.5(8) . . ?
C32 C33 C34 119.6(8) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C34 N6 H32A 120.0 . . ?
C34 N6 H32B 120.0 . . ?
H32A N6 H32B 120.0 . . ?
C23 C25 H14A 109.5 . . ?
C23 C25 H14B 109.5 . . ?
H14A C25 H14B 109.5 . . ?
C23 C25 H14C 109.5 . . ?
H14A C25 H14C 109.5 . . ?
H14B C25 H14C 109.5 . . ?
C11 C14 H24A 109.5 . . ?
C11 C14 H24B 109.5 . . ?
H24A C14 H24B 109.5 . . ?
C11 C14 H24C 109.5 . . ?
H24A C14 H24C 109.5 . . ?
H24B C14 H24C 109.5 . . ?
C21 C24 H15A 109.5 . . ?
C21 C24 H15B 109.5 . . ?
H15A C24 H15B 109.5 . . ?
C21 C24 H15C 109.5 . . ?
H15A C24 H15C 109.5 . . ?
H15B C24 H15C 109.5 . . ?
C13 C15 H25A 109.5 . . ?
C13 C15 H25B 109.5 . . ?
H25A C15 H25B 109.5 . . ?
C13 C15 H25C 109.5 . . ?
H25A C15 H25C 109.5 . . ?
H25B C15 H25C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C1 1.910(9) . ?
Re1 C2 1.926(9) . ?
Re1 C3 1.949(12) . ?
Re1 N3 2.207(7) . ?
Re1 N1 2.212(7) . ?
Re1 N5 2.236(7) . ?
C2 O2 1.135(11) . ?
N3 C23 1.314(11) . ?
N3 N4 1.355(9) . ?
N1 C11 1.351(11) . ?
N1 N2 1.357(10) . ?
N5 C31 1.316(11) . ?
N5 C35 1.342(11) . ?
O1 C1 1.162(11) . ?
O3 C3 1.168(13) . ?
N4 C21 1.350(12) . ?
N4 H112 0.87(2) . ?
N2 C13 1.347(11) . ?
N2 H2 0.8600 . ?
C35 C34 1.396(11) . ?
C35 H331 0.9300 . ?
C31 C32 1.385(12) . ?
C31 H35 0.9300 . ?
C34 N6 1.363(13) . ?
C34 C33 1.394(14) . ?
C13 C12 1.370(14) . ?
C13 C15 1.477(14) . ?
C23 C22 1.391(12) . ?
C23 C25 1.493(12) . ?
C32 C33 1.359(14) . ?
C32 H34 0.9300 . ?
C12 C11 1.418(13) . ?
C12 H22 0.9300 . ?
C21 C22 1.347(13) . ?
C21 C24 1.487(12) . ?
C22 H12 0.9300 . ?
C11 C14 1.480(15) . ?
C33 H33 0.9300 . ?
N6 H32A 0.8600 . ?
N6 H32B 0.8600 . ?
C25 H14A 0.9600 . ?
C25 H14B 0.9600 . ?
C25 H14C 0.9600 . ?
C14 H24A 0.9600 . ?
C14 H24B 0.9600 . ?
C14 H24C 0.9600 . ?
C24 H15A 0.9600 . ?
C24 H15B 0.9600 . ?
C24 H15C 0.9600 . ?
C15 H25A 0.9600 . ?
C15 H25B 0.9600 . ?
C15 H25C 0.9600 . ?
O10 H100 0.58(16) . ?
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
_geom_hbond_site_symmetry_A
O10 H100 Br1 0.58(16) 2.96(16) 3.520(9) 165(22) 1_566
N6 H32A Br1 0.86 2.64 3.440(8) 154.9 1_556
N6 H32B Br1 0.86 2.87 3.614(10) 145.9 2_766
N4 H112 O10 0.87(2) 2.00(4) 2.803(11) 153(7) .
N2 H2 Br1 0.86 2.79 3.534(8) 146.1 2_766
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
_geom_torsion_publ_flag
C1 Re1 N3 C23 48.9(8) . . . . ?
C2 Re1 N3 C23 -40.8(8) . . . . ?
N1 Re1 N3 C23 141.4(7) . . . . ?
N5 Re1 N3 C23 -129.7(7) . . . . ?
C1 Re1 N3 N4 -124.6(6) . . . . ?
C2 Re1 N3 N4 145.7(6) . . . . ?
N1 Re1 N3 N4 -32.1(6) . . . . ?
N5 Re1 N3 N4 56.9(6) . . . . ?
C1 Re1 N1 C11 39.9(8) . . . . ?
C3 Re1 N1 C11 128.2(8) . . . . ?
N3 Re1 N1 C11 -52.2(8) . . . . ?
N5 Re1 N1 C11 -137.5(8) . . . . ?
C1 Re1 N1 N2 -131.6(6) . . . . ?
C3 Re1 N1 N2 -43.4(6) . . . . ?
N3 Re1 N1 N2 136.3(6) . . . . ?
N5 Re1 N1 N2 50.9(6) . . . . ?
C2 Re1 N5 C31 -70.8(7) . . . . ?
C3 Re1 N5 C31 -156.0(6) . . . . ?
N3 Re1 N5 C31 24.6(6) . . . . ?
N1 Re1 N5 C31 109.2(6) . . . . ?
C2 Re1 N5 C35 104.4(6) . . . . ?
C3 Re1 N5 C35 19.3(6) . . . . ?
N3 Re1 N5 C35 -160.2(6) . . . . ?
N1 Re1 N5 C35 -75.6(6) . . . . ?
C23 N3 N4 C21 0.2(9) . . . . ?
Re1 N3 N4 C21 175.0(5) . . . . ?
C11 N1 N2 C13 0.6(10) . . . . ?
Re1 N1 N2 C13 174.2(6) . . . . ?
C31 N5 C35 C34 -1.7(12) . . . . ?
Re1 N5 C35 C34 -177.2(6) . . . . ?
C35 N5 C31 C32 2.4(12) . . . . ?
Re1 N5 C31 C32 177.7(6) . . . . ?
N5 C35 C34 N6 -178.6(9) . . . . ?
N5 C35 C34 C33 -0.5(12) . . . . ?
N1 N2 C13 C12 -0.3(11) . . . . ?
N1 N2 C13 C15 -177.9(9) . . . . ?
N4 N3 C23 C22 0.1(9) . . . . ?
Re1 N3 C23 C22 -174.0(5) . . . . ?
N4 N3 C23 C25 -178.9(8) . . . . ?
Re1 N3 C23 C25 7.0(12) . . . . ?
N5 C31 C32 C33 -0.8(13) . . . . ?
N2 C13 C12 C11 -0.1(10) . . . . ?
C15 C13 C12 C11 177.2(11) . . . . ?
N3 N4 C21 C22 -0.4(9) . . . . ?
N3 N4 C21 C24 -179.9(8) . . . . ?
N4 C21 C22 C23 0.5(9) . . . . ?
C24 C21 C22 C23 179.9(9) . . . . ?
N3 C23 C22 C21 -0.4(10) . . . . ?
C25 C23 C22 C21 178.5(8) . . . . ?
N2 N1 C11 C12 -0.6(10) . . . . ?
Re1 N1 C11 C12 -173.2(6) . . . . ?
N2 N1 C11 C14 178.4(9) . . . . ?
Re1 N1 C11 C14 5.9(14) . . . . ?
C13 C12 C11 N1 0.5(10) . . . . ?
C13 C12 C11 C14 -178.6(9) . . . . ?
C31 C32 C33 C34 -1.6(13) . . . . ?
N6 C34 C33 C32 -179.9(9) . . . . ?
C35 C34 C33 C32 2.1(12) . . . . ?
