#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/54/4325425.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_4325425
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 Ni O8 Re2 n6'
_chemical_formula_weight         1867.51
_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                 95.935(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2201(11)
_cell_length_b                   16.3950(11)
_cell_length_c                   34.675(3)
_cell_measurement_temperature    293(2)
_cell_volume                     6344.4(9)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            64148
_diffrn_reflns_theta_full        28.12
_diffrn_reflns_theta_max         28.12
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    9.185
_exptl_absorpt_correction_T_max  0.399
_exptl_absorpt_correction_T_min  0.330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_description       'hexagonal plates'
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         7697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0362P)²+20.0028P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                6204
_reflns_number_total             7697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200531s_si_004.cif
_cod_data_source_block           Compound3_re2ni
_cod_original_cell_volume        6344.5(9)
_cod_original_formula_sum        'C42 H80 Br8 n6 Ni O8 Re2'
_cod_database_code               4325425
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 0.687371(15) -0.098715(11) 0.371091(5) 0.04810(7) Uani 1 1 d .
Ni1 ni 0.5000 0.09004(4) 0.2500 0.04281(17) Uani 1 2 d S
Br3 Br 0.85309(5) -0.19691(3) 0.376334(18) 0.07158(16) Uani 1 1 d .
Br2 Br 0.63232(6) -0.11862(4) 0.437032(17) 0.07719(17) Uani 1 1 d .
Br4 Br 0.82429(5) 0.01615(4) 0.39129(2) 0.08095(18) Uani 1 1 d .
Br1 Br 0.54081(6) -0.20379(4) 0.34509(2) 0.08709(19) Uani 1 1 d .
O3 O 0.6301(3) -0.00373(19) 0.26226(9) 0.0531(7) Uani 1 1 d .
O1 O 0.7115(3) -0.0745(2) 0.31342(10) 0.0565(8) Uani 1 1 d .
O4 O 0.4909(3) 0.07521(18) 0.30963(9) 0.0488(7) Uani 1 1 d .
O2 O 0.5570(3) -0.0103(2) 0.35717(9) 0.0560(8) Uani 1 1 d .
N2 n 1.2644(3) 0.5323(3) 0.09228(13) 0.0596(10) Uani 1 1 d .
N1 n 0.6310(3) 0.1758(2) 0.25339(11) 0.0536(9) Uani 1 1 d .
C7 C 0.5546(4) 0.0186(3) 0.32303(13) 0.0454(9) Uani 1 1 d .
C6 C 0.6379(4) -0.0227(3) 0.29660(13) 0.0458(9) Uani 1 1 d .
C20 C 1.1518(4) 0.5843(3) 0.08954(15) 0.0554(11) Uani 1 1 d .
H20A H 1.1755 0.6412 0.0915 0.066 Uiso 1 1 calc R
H20B H 1.1086 0.5721 0.1117 0.066 Uiso 1 1 calc R
C21 C 1.0665(4) 0.5735(3) 0.05287(17) 0.0651(13) Uani 1 1 d .
H21A H 1.1053 0.5911 0.0306 0.078 Uiso 1 1 calc R
H21B H 1.0456 0.5164 0.0495 0.078 Uiso 1 1 calc R
C16 C 1.3447(5) 0.5591(4) 0.12741(16) 0.0718(15) Uani 1 1 d .
H16A H 1.3597 0.6171 0.1252 0.086 Uiso 1 1 calc R
H16B H 1.4210 0.5313 0.1274 0.086 Uiso 1 1 calc R
C12 C 1.2270(5) 0.4432(3) 0.0948(2) 0.0732(16) Uani 1 1 d .
H12A H 1.1769 0.4377 0.1159 0.088 Uiso 1 1 calc R
H12B H 1.1787 0.4288 0.0710 0.088 Uiso 1 1 calc R
C8 C 1.3327(5) 0.5421(4) 0.05733(17) 0.0777(17) Uani 1 1 d .
H8A H 1.4061 0.5106 0.0617 0.093 Uiso 1 1 calc R
H8B H 1.2853 0.5182 0.0352 0.093 Uiso 1 1 calc R
C9 C 1.3645(6) 0.6258(5) 0.0470(2) 0.097(2) Uani 1 1 d .
H9A H 1.4117 0.6518 0.0686 0.116 Uiso 1 1 calc R
H9B H 1.2928 0.6579 0.0403 0.116 Uiso 1 1 calc R
C10 C 1.4406(10) 0.6181(7) 0.0106(3) 0.140(4) Uani 1 1 d .
H10A H 1.5131 0.5876 0.0186 0.169 Uiso 1 1 calc R
H10B H 1.3944 0.5866 -0.0094 0.169 Uiso 1 1 calc R
C13 C 1.3296(6) 0.3829(4) 0.1013(3) 0.106(3) Uani 1 1 d .
H13A H 1.3873 0.4025 0.1220 0.128 Uiso 1 1 calc R
H13B H 1.3698 0.3787 0.0779 0.128 Uiso 1 1 calc R
C17 C 1.2968(6) 0.5435(6) 0.16603(19) 0.100(2) Uani 1 1 d .
H17A H 1.2750 0.4865 0.1679 0.120 Uiso 1 1 calc R
H17B H 1.2255 0.5761 0.1679 0.120 Uiso 1 1 calc R
N3 n 0.7258(5) 0.2835(4) 0.23487(18) 0.0999(18) Uani 1 1 d .
H3A H 0.7439 0.3240 0.2208 0.120 Uiso 1 1 calc R
C22 C 0.9540(5) 0.6234(4) 0.05574(17) 0.0722(15) Uani 1 1 d .
H22A H 0.9754 0.6804 0.0594 0.087 Uiso 1 1 calc R
H22B H 0.9156 0.6057 0.0781 0.087 Uiso 1 1 calc R
C2 C 0.6394(6) 0.2292(4) 0.22586(18) 0.0814(18) Uani 1 1 d .
H2A H 0.5904 0.2292 0.2025 0.098 Uiso 1 1 calc R
C23 C 0.8660(6) 0.6140(4) 0.0190(2) 0.096(2) Uani 1 1 d .
H23A H 0.7961 0.6467 0.0214 0.143 Uiso 1 1 calc R
H23B H 0.8431 0.5578 0.0158 0.143 Uiso 1 1 calc R
H23C H 0.9039 0.6317 -0.0032 0.143 Uiso 1 1 calc R
C4 C 0.7781(9) 0.2641(6) 0.2691(3) 0.145(4) Uani 1 1 d .
H4A H 0.8430 0.2900 0.2828 0.174 Uiso 1 1 calc R
C5 C 0.7173(8) 0.1975(5) 0.2805(2) 0.118(3) Uani 1 1 d .
H5A H 0.7341 0.1710 0.3041 0.141 Uiso 1 1 calc R
C14 C 1.2826(7) 0.2950(5) 0.1124(3) 0.125(3) Uani 1 1 d .
H14A H 1.3503 0.2584 0.1175 0.150 Uiso 1 1 calc R
H14B H 1.2432 0.2992 0.1360 0.150 Uiso 1 1 calc R
C15 C 1.2035(10) 0.2629(7) 0.0833(3) 0.151(4) Uiso 1 1 d .
H15A H 1.1780 0.2099 0.0908 0.227 Uiso 1 1 calc R
H15B H 1.2423 0.2584 0.0599 0.227 Uiso 1 1 calc R
H15C H 1.1351 0.2981 0.0787 0.227 Uiso 1 1 calc R
C18 C 1.3918(11) 0.5653(8) 0.1990(4) 0.169(4) Uiso 1 1 d .
H18A H 1.3567 0.5735 0.2231 0.203 Uiso 1 1 calc R
H18B H 1.4355 0.6140 0.1930 0.203 Uiso 1 1 calc R
C19 C 1.4795(15) 0.4836(11) 0.2012(5) 0.264(8) Uiso 1 1 d .
H19A H 1.5420 0.4897 0.2221 0.396 Uiso 1 1 calc R
H19B H 1.5143 0.4777 0.1772 0.396 Uiso 1 1 calc R
H19C H 1.4329 0.4360 0.2056 0.396 Uiso 1 1 calc R
C11 C 1.4702(12) 0.6855(8) -0.0042(3) 0.183(5) Uani 1 1 d .
H11A H 1.5156 0.6747 -0.0256 0.275 Uiso 1 1 calc R
H11B H 1.5180 0.7168 0.0150 0.275 Uiso 1 1 calc R
H11C H 1.3993 0.7156 -0.0131 0.275 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'
Ni Ni 0.3393 1.1124 '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 78.61(12) . .
O2 Re1 Br2 94.03(8) . .
O1 Re1 Br2 172.25(8) . .
O2 Re1 Br3 169.84(8) . .
O1 Re1 Br3 91.35(8) . .
Br2 Re1 Br3 96.07(2) . .
O2 Re1 Br4 86.37(10) . .
O1 Re1 Br4 89.34(10) . .
Br2 Re1 Br4 92.64(3) . .
Br3 Re1 Br4 91.99(2) . .
O2 Re1 Br1 88.61(10) . .
O1 Re1 Br1 86.01(10) . .
Br2 Re1 Br1 91.43(3) . .
Br3 Re1 Br1 92.29(2) . .
Br4 Re1 Br1 173.75(2) . .
N1 ni1 N1 92.3(2) . 2_655
N1 ni1 O4 91.64(14) . 2_655
N1 ni1 O4 97.60(14) 2_655 2_655
N1 ni1 O4 97.60(14) . .
N1 ni1 O4 91.64(14) 2_655 .
O4 ni1 O4 166.67(17) 2_655 .
N1 ni1 O3 171.20(14) . 2_655
N1 ni1 O3 90.62(15) 2_655 2_655
O4 ni1 O3 79.74(11) 2_655 2_655
O4 ni1 O3 90.62(12) . 2_655
N1 ni1 O3 90.62(15) . .
N1 ni1 O3 171.20(14) 2_655 .
O4 ni1 O3 90.62(12) 2_655 .
O4 ni1 O3 79.74(11) . .
O3 ni1 O3 87.75(18) 2_655 .
C6 O3 ni1 110.8(3) . .
C6 O1 Re1 114.9(3) . .
C7 O4 ni1 111.9(3) . .
C7 O2 Re1 114.9(3) . .
C16 n2 C8 107.9(4) . .
C16 n2 C20 108.1(4) . .
C8 n2 C20 112.2(4) . .
C16 n2 C12 112.3(5) . .
C8 n2 C12 108.3(4) . .
C20 n2 C12 108.1(3) . .
C2 n1 C5 103.6(5) . .
C2 n1 Ni1 121.9(4) . .
C5 n1 Ni1 134.3(4) . .
O4 C7 O2 125.9(4) . .
O4 C7 C6 118.2(4) . .
O2 C7 C6 115.9(4) . .
O3 C6 O1 126.0(4) . .
O3 C6 C7 118.9(4) . .
O1 C6 C7 115.1(4) . .
N2 C20 C21 115.7(4) . .
C22 C21 C20 109.8(4) . .
N2 C16 C17 115.4(5) . .
C13 C12 n2 115.1(5) . .
C9 C8 n2 116.8(5) . .
C8 C9 C10 106.3(7) . .
C11 C10 C9 115.6(10) . .
C12 C13 C14 111.1(6) . .
C16 C17 C18 109.7(7) . .
C4 n3 C2 107.3(6) . .
C21 C22 C23 111.1(5) . .
N1 C2 n3 112.6(6) . .
N3 C4 C5 105.4(6) . .
N1 C5 C4 111.1(7) . .
C15 C14 C13 111.8(9) . .
C17 C18 C19 102.2(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 O2 2.081(3) .
Re1 O1 2.084(3) .
Re1 Br2 2.4512(6) .
Re1 Br3 2.4520(5) .
Re1 Br4 2.4849(6) .
Re1 Br1 2.4856(6) .
Ni1 n1 2.028(4) .
Ni1 n1 2.028(4) 2_655
Ni1 O4 2.095(3) 2_655
Ni1 O4 2.095(3) .
Ni1 O3 2.133(3) 2_655
Ni1 O3 2.133(3) .
O3 C6 1.225(5) .
O1 C6 1.282(5) .
O4 C7 1.233(5) .
O2 C7 1.273(5) .
N2 C16 1.504(7) .
N2 C8 1.508(7) .
N2 C20 1.519(6) .
N2 C12 1.524(7) .
N1 C2 1.306(7) .
N1 C5 1.326(8) .
C7 C6 1.532(6) .
C20 C21 1.521(7) .
C21 C22 1.516(7) .
C16 C17 1.516(8) .
C12 C13 1.517(8) .
C8 C9 1.471(9) .
C9 C10 1.601(11) .
C10 C11 1.276(12) .
C13 C14 1.596(11) .
C17 C18 1.522(13) .
N3 C4 1.309(9) .
N3 C2 1.330(7) .
C22 C23 1.538(8) .
C4 C5 1.366(10) .
C14 C15 1.379(12) .
C18 C19 1.659(18) .
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 2.13 2.993(6) 179.2 4_655
