#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/54/4325426.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_4325426
loop_
_publ_author_name
'José Martínez-Lillo'
'Teresa F. Mastropietro'
'Giovanni De Munno'
'Francesc Lloret'
'Miguel Julve'
'Juan Faus'
_publ_section_title
;
 Enhancing the Magnetic Coupling of Oxalato-Bridged ReIV2MII (M = Mn, Co,
 ni, and Cu) Trinuclear Complexes via Peripheral Halide Ligand Effects
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5731
_journal_page_last               5739
_journal_paper_doi               10.1021/ic200531s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C42 H80 Br8 Cu O8 Re2 n6'
_chemical_formula_weight         1872.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.301(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2120(6)
_cell_length_b                   16.3081(6)
_cell_length_c                   34.7810(13)
_cell_measurement_temperature    293(2)
_cell_volume                     6321.2(5)
_computing_cell_refinement       'Bruker-Nonius X8 APEX'
_computing_data_collection       'Bruker-Nonius X8 APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            30011
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    9.257
_exptl_absorpt_correction_T_max  0.4579
_exptl_absorpt_correction_T_min  0.4030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             3588
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         7886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0274P)²+15.4307P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                5949
_reflns_number_total             7886
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200531s_si_005.cif
_cod_data_source_block           Compound4_re2cu
_cod_original_formula_sum        'C42 H80 Br8 Cu n6 O8 Re2'
_cod_database_code               4325426
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Re1 Re 0.684676(15) -0.101600(11) 0.371377(5) 0.04561(6) Uani 1 1 d .
Cu1 Cu 0.5000 0.09791(4) 0.2500 0.04161(16) Uani 1 2 d S
Br3 Br 0.85449(5) -0.19746(3) 0.374579(16) 0.06512(14) Uani 1 1 d .
Br2 Br 0.63519(5) -0.12677(4) 0.437137(15) 0.07226(16) Uani 1 1 d .
Br4 Br 0.81927(5) 0.01494(4) 0.39225(2) 0.07713(17) Uani 1 1 d .
Br1 Br 0.54178(6) -0.20880(4) 0.34433(2) 0.08309(18) Uani 1 1 d .
O3 O 0.6230(3) 0.00679(19) 0.26551(9) 0.0508(7) Uani 1 1 d .
O1 O 0.7029(3) -0.07181(19) 0.31377(9) 0.0512(7) Uani 1 1 d .
O4 O 0.4824(3) 0.0774(2) 0.31610(9) 0.0552(8) Uani 1 1 d .
O2 O 0.5507(3) -0.0158(2) 0.36003(9) 0.0541(8) Uani 1 1 d .
N2 n 1.2683(3) 0.5305(2) 0.09214(11) 0.0522(9) Uani 1 1 d .
N1 n 0.6282(3) 0.1816(2) 0.25313(11) 0.0495(9) Uani 1 1 d .
C7 C 0.5459(4) 0.0203(3) 0.32685(12) 0.0452(10) Uani 1 1 d .
C6 C 0.6303(4) -0.0173(3) 0.29930(12) 0.0440(10) Uani 1 1 d .
C20 C 1.1566(4) 0.5842(3) 0.08906(14) 0.0539(11) Uani 1 1 d .
H20A H 1.1153 0.5748 0.1118 0.065 Uiso 1 1 calc R
H20B H 1.1817 0.6411 0.0896 0.065 Uiso 1 1 calc R
C21 C 1.0684(4) 0.5709(3) 0.05350(16) 0.0629(13) Uani 1 1 d .
H21A H 1.1055 0.5857 0.0306 0.076 Uiso 1 1 calc R
H21B H 1.0463 0.5134 0.0515 0.076 Uiso 1 1 calc R
C16 C 1.3516(5) 0.5570(4) 0.12702(15) 0.0688(14) Uani 1 1 d .
H16A H 1.4261 0.5268 0.1271 0.083 Uiso 1 1 calc R
H16B H 1.3702 0.6146 0.1241 0.083 Uiso 1 1 calc R
C12 C 1.2296(4) 0.4415(3) 0.09590(18) 0.0677(14) Uani 1 1 d .
H12A H 1.1809 0.4377 0.1172 0.081 Uiso 1 1 calc R
H12B H 1.1793 0.4263 0.0725 0.081 Uiso 1 1 calc R
C8 C 1.3351(5) 0.5373(4) 0.05690(15) 0.0664(14) Uani 1 1 d .
H8A H 1.4086 0.5058 0.0617 0.080 Uiso 1 1 calc R
H8B H 1.2867 0.5118 0.0353 0.080 Uiso 1 1 calc R
C9 C 1.3667(6) 0.6206(4) 0.04506(18) 0.0831(18) Uani 1 1 d .
H9A H 1.4125 0.6486 0.0664 0.100 Uiso 1 1 calc R
H9B H 1.2945 0.6520 0.0375 0.100 Uiso 1 1 calc R
C10 C 1.4429(7) 0.6130(4) 0.0102(2) 0.106(2) Uani 1 1 d .
H10A H 1.5184 0.5864 0.0190 0.127 Uiso 1 1 calc R
H10B H 1.4005 0.5784 -0.0094 0.127 Uiso 1 1 calc R
C13 C 1.3308(5) 0.3800(4) 0.1026(2) 0.098(2) Uani 1 1 d .
H13A H 1.3885 0.3986 0.1236 0.117 Uiso 1 1 calc R
H13B H 1.3717 0.3758 0.0795 0.117 Uiso 1 1 calc R
C17 C 1.3057(5) 0.5455(5) 0.16563(17) 0.094(2) Uani 1 1 d .
H17A H 1.2787 0.4895 0.1681 0.112 Uiso 1 1 calc R
H17B H 1.2380 0.5817 0.1677 0.112 Uiso 1 1 calc R
N3 n 0.7272(5) 0.2855(3) 0.23437(15) 0.0829(15) Uani 1 1 d .
H3A H 0.7476 0.3254 0.2203 0.099 Uiso 1 1 calc R
C22 C 0.9575(5) 0.6223(3) 0.05582(16) 0.0654(14) Uani 1 1 d .
H22A H 0.9801 0.6797 0.0580 0.078 Uiso 1 1 calc R
H22B H 0.9210 0.6075 0.0789 0.078 Uiso 1 1 calc R
C2 C 0.6381(5) 0.2343(4) 0.22566(16) 0.0725(16) Uani 1 1 d .
H2A H 0.5880 0.2355 0.2025 0.087 Uiso 1 1 calc R
C23 C 0.8661(6) 0.6105(4) 0.02034(19) 0.0878(19) Uani 1 1 d .
H23A H 0.7964 0.6433 0.0230 0.132 Uiso 1 1 calc R
H23B H 0.8434 0.5538 0.0182 0.132 Uiso 1 1 calc R
H23C H 0.9011 0.6269 -0.0024 0.132 Uiso 1 1 calc R
C4 C 0.7797(7) 0.2642(5) 0.2689(2) 0.133(4) Uani 1 1 d .
H4A H 0.8464 0.2889 0.2824 0.159 Uiso 1 1 calc R
C5 C 0.7177(7) 0.1998(5) 0.2806(2) 0.113(3) Uani 1 1 d .
H5A H 0.7343 0.1723 0.3040 0.135 Uiso 1 1 calc R
C14 C 1.2819(7) 0.2937(5) 0.1127(3) 0.117(3) Uani 1 1 d .
H14A H 1.3492 0.2567 0.1186 0.140 Uiso 1 1 calc R
H14B H 1.2412 0.2985 0.1358 0.140 Uiso 1 1 calc R
C15 C 1.2020(9) 0.2590(5) 0.0830(3) 0.141(4) Uani 1 1 d .
H15A H 1.1771 0.2059 0.0909 0.212 Uiso 1 1 calc R
H15B H 1.2415 0.2538 0.0600 0.212 Uiso 1 1 calc R
H15C H 1.1331 0.2939 0.0779 0.212 Uiso 1 1 calc R
C18 C 1.4055(9) 0.5646(6) 0.1980(3) 0.150(3) Uiso 1 1 d .
H18A H 1.3727 0.5736 0.2223 0.180 Uiso 1 1 calc R
H18B H 1.4502 0.6129 0.1919 0.180 Uiso 1 1 calc R
C19 C 1.4901(12) 0.4839(9) 0.2003(4) 0.235(6) Uiso 1 1 d .
H19A H 1.5530 0.4898 0.2212 0.353 Uiso 1 1 calc R
H19B H 1.5247 0.4777 0.1764 0.353 Uiso 1 1 calc R
H19C H 1.4429 0.4364 0.2047 0.353 Uiso 1 1 calc R
C11 C 1.4667(8) 0.6887(6) -0.0062(3) 0.136(3) Uiso 1 1 d .
H11A H 1.5121 0.6803 -0.0277 0.204 Uiso 1 1 calc R
H11B H 1.5119 0.7224 0.0128 0.204 Uiso 1 1 calc R
H11C H 1.3924 0.7155 -0.0150 0.204 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'
Cu Cu 0.3201 1.2651 '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'
Br Br -0.2901 2.4595 '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
O2 Re1 O1 78.74(11) . .
O2 Re1 Br2 93.30(8) . .
O1 Re1 Br2 171.75(8) . .
O2 Re1 Br3 170.61(8) . .
O1 Re1 Br3 91.98(8) . .
Br2 Re1 Br3 96.03(2) . .
O2 Re1 Br4 86.76(10) . .
O1 Re1 Br4 88.98(9) . .
Br2 Re1 Br4 92.75(2) . .
Br3 Re1 Br4 91.76(2) . .
O2 Re1 Br1 88.78(10) . .
O1 Re1 Br1 85.84(9) . .
Br2 Re1 Br1 91.89(2) . .
Br3 Re1 Br1 91.93(2) . .
Br4 Re1 Br1 173.74(2) . .
N1 Cu1 n1 92.7(2) . 2_655
N1 Cu1 O3 167.19(13) . 2_655
N1 Cu1 O3 91.25(14) 2_655 2_655
N1 Cu1 O3 91.25(14) . .
N1 Cu1 O3 167.19(13) 2_655 .
O3 Cu1 O3 87.59(18) 2_655 .
N1 Cu1 O4 90.77(13) . 2_655
N1 Cu1 O4 100.55(14) 2_655 2_655
O3 Cu1 O4 76.52(11) 2_655 2_655
O3 Cu1 O4 91.59(12) . 2_655
N1 Cu1 O4 100.55(14) . .
N1 Cu1 O4 90.77(13) 2_655 .
O3 Cu1 O4 91.59(12) 2_655 .
O3 Cu1 O4 76.52(11) . .
O4 Cu1 O4 163.63(16) 2_655 .
C6 O3 Cu1 116.9(3) . .
C6 O1 Re1 114.6(3) . .
C7 O4 Cu1 107.6(3) . .
C7 O2 Re1 116.0(3) . .
C8 n2 C16 108.2(4) . .
C8 n2 C20 112.3(4) . .
C16 n2 C20 108.9(4) . .
C8 n2 C12 108.1(4) . .
C16 n2 C12 111.1(4) . .
C20 n2 C12 108.3(3) . .
C2 n1 C5 105.1(5) . .
C2 n1 Cu1 122.5(3) . .
C5 n1 Cu1 132.4(4) . .
O4 C7 O2 126.5(4) . .
O4 C7 C6 119.7(4) . .
O2 C7 C6 113.9(4) . .
O3 C6 O1 124.9(4) . .
O3 C6 C7 118.9(4) . .
O1 C6 C7 116.2(4) . .
C21 C20 n2 115.8(4) . .
C22 C21 C20 110.2(4) . .
C17 C16 n2 116.1(5) . .
C13 C12 n2 115.4(4) . .
C9 C8 n2 116.8(4) . .
C8 C9 C10 108.2(5) . .
C11 C10 C9 113.1(7) . .
C12 C13 C14 110.8(5) . .
C16 C17 C18 109.8(6) . .
C2 n3 C4 107.1(5) . .
C21 C22 C23 111.7(4) . .
N1 C2 n3 112.1(5) . .
N3 C4 C5 106.6(6) . .
N1 C5 C4 109.1(6) . .
C15 C14 C13 113.9(8) . .
C17 C18 C19 104.4(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 O2 2.059(3) .
Re1 O1 2.093(3) .
Re1 Br2 2.4466(5) .
Re1 Br3 2.4565(5) .
Re1 Br4 2.4852(6) .
Re1 Br1 2.4855(6) .
Cu1 n1 1.977(4) .
Cu1 n1 1.977(4) 2_655
Cu1 O3 2.059(3) 2_655
Cu1 O3 2.059(3) .
Cu1 O4 2.353(3) 2_655
Cu1 O4 2.353(3) .
O3 C6 1.233(5) .
O1 C6 1.271(5) .
O4 C7 1.206(5) .
O2 C7 1.292(5) .
N2 C8 1.509(6) .
N2 C16 1.511(6) .
N2 C20 1.521(6) .
N2 C12 1.525(6) .
N1 C2 1.299(6) .
N1 C5 1.340(7) .
C7 C6 1.546(6) .
C20 C21 1.512(7) .
C21 C22 1.509(7) .
C16 C17 1.502(7) .
C12 C13 1.514(7) .
C8 C9 1.473(8) .
C9 C10 1.561(9) .
C10 C11 1.399(10) .
C13 C14 1.565(10) .
C17 C18 1.530(11) .
N3 C2 1.311(6) .
N3 C4 1.324(8) .
C22 C23 1.527(8) .
C4 C5 1.348(9) .
C14 C15 1.409(11) .
C18 C19 1.619(15) .
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
N3 H3A O1 0.86 2.16 3.020(5) 178.3 4_655
