#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/54/4325423.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_4325423
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 Mn O8 Re2 n6'
_chemical_formula_weight         1863.74
_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                 96.6510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1814(4)
_cell_length_b                   16.5320(4)
_cell_length_c                   35.0505(11)
_cell_measurement_temperature    293(2)
_cell_volume                     6435.5(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            48843
_diffrn_reflns_theta_full        29.87
_diffrn_reflns_theta_max         29.87
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    8.958
_exptl_absorpt_correction_T_max  0.378
_exptl_absorpt_correction_T_min  0.299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_description       'hexagonal pltes'
_exptl_crystal_F_000             3572
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.288
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         9235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0371
_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)+(0.0334P)²+18.3699P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                7086
_reflns_number_total             9235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200531s_si_002.cif
_cod_data_source_block           Compound1_re2mn
_cod_original_formula_sum        'C42 H80 Br8 Mn n6 O8 Re2'
_cod_database_code               4325423
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 0.685763(14) -0.099640(10) 0.374831(5) 0.04661(6) Uani 1 1 d .
Mn1 Mn 0.5000 0.09394(5) 0.2500 0.04357(19) Uani 1 2 d S
Br3 Br 0.85181(5) -0.19735(3) 0.380693(17) 0.07008(15) Uani 1 1 d .
Br2 Br 0.62753(5) -0.12083(4) 0.439267(15) 0.07385(16) Uani 1 1 d .
Br4 Br 0.82303(5) 0.01377(3) 0.396458(19) 0.07555(16) Uani 1 1 d .
Br1 Br 0.53928(6) -0.20302(4) 0.34703(2) 0.08578(18) Uani 1 1 d .
O3 O 0.6361(3) -0.00396(19) 0.26713(9) 0.0573(8) Uani 1 1 d .
O1 O 0.7140(3) -0.07438(18) 0.31826(9) 0.0541(7) Uani 1 1 d .
O4 O 0.4889(3) 0.07189(18) 0.31256(8) 0.0521(7) Uani 1 1 d .
O2 O 0.5550(3) -0.01193(19) 0.36012(9) 0.0547(7) Uani 1 1 d .
N2 n 1.2666(3) 0.5323(2) 0.09156(11) 0.0542(9) Uani 1 1 d .
N1 n 0.6407(4) 0.1841(2) 0.25067(11) 0.0589(10) Uani 1 1 d .
C7 C 0.5530(3) 0.0169(2) 0.32621(11) 0.0441(9) Uani 1 1 d .
C6 C 0.6417(4) -0.0229(2) 0.30124(12) 0.0460(9) Uani 1 1 d .
C20 C 1.1547(4) 0.5843(3) 0.08844(14) 0.0528(10) Uani 1 1 d .
H20A H 1.1123 0.5734 0.1105 0.063 Uiso 1 1 calc R
H20B H 1.1795 0.6406 0.0900 0.063 Uiso 1 1 calc R
C21 C 1.0675(4) 0.5735(3) 0.05260(16) 0.0635(12) Uani 1 1 d .
H21A H 1.0458 0.5169 0.0495 0.076 Uiso 1 1 calc R
H21B H 1.1053 0.5901 0.0303 0.076 Uiso 1 1 calc R
C16 C 1.3508(5) 0.5585(4) 0.12663(14) 0.0673(13) Uani 1 1 d .
H16A H 1.4259 0.5290 0.1268 0.081 Uiso 1 1 calc R
H16B H 1.3687 0.6155 0.1241 0.081 Uiso 1 1 calc R
C12 C 1.2286(4) 0.4439(3) 0.09486(18) 0.0720(15) Uani 1 1 d .
H12A H 1.1781 0.4397 0.1155 0.086 Uiso 1 1 calc R
H12B H 1.1801 0.4287 0.0712 0.086 Uiso 1 1 calc R
C8 C 1.3336(4) 0.5407(4) 0.05649(15) 0.0697(14) Uani 1 1 d .
H8A H 1.4063 0.5083 0.0607 0.084 Uiso 1 1 calc R
H8B H 1.2838 0.5177 0.0347 0.084 Uiso 1 1 calc R
C9 C 1.3680(6) 0.6232(4) 0.04605(18) 0.0869(18) Uani 1 1 d .
H9A H 1.4162 0.6487 0.0675 0.104 Uiso 1 1 calc R
H9B H 1.2967 0.6559 0.0392 0.104 Uiso 1 1 calc R
C10 C 1.4432(8) 0.6153(5) 0.0106(2) 0.110(2) Uani 1 1 d .
H10A H 1.5164 0.5853 0.0186 0.132 Uiso 1 1 calc R
H10B H 1.3966 0.5846 -0.0095 0.132 Uiso 1 1 calc R
C13 C 1.3313(6) 0.3839(4) 0.1024(3) 0.107(3) Uani 1 1 d .
H13A H 1.3892 0.4043 0.1229 0.129 Uiso 1 1 calc R
H13B H 1.3719 0.3788 0.0795 0.129 Uiso 1 1 calc R
C17 C 1.3036(6) 0.5457(5) 0.16466(16) 0.093(2) Uani 1 1 d .
H17A H 1.2801 0.4896 0.1671 0.111 Uiso 1 1 calc R
H17B H 1.2331 0.5793 0.1661 0.111 Uiso 1 1 calc R
N3 n 0.7285(5) 0.2906(3) 0.23094(17) 0.1013(18) Uani 1 1 d .
H3A H 0.7430 0.3310 0.2168 0.122 Uiso 1 1 calc R
C22 C 0.9553(5) 0.6234(3) 0.05519(16) 0.0662(13) Uani 1 1 d .
H22A H 0.9774 0.6800 0.0582 0.079 Uiso 1 1 calc R
H22B H 0.9184 0.6070 0.0777 0.079 Uiso 1 1 calc R
C2 C 0.6459(6) 0.2351(4) 0.22294(17) 0.0819(17) Uani 1 1 d .
H2A H 0.5963 0.2326 0.1998 0.098 Uiso 1 1 calc R
C23 C 0.8649(6) 0.6135(4) 0.01971(19) 0.0871(18) Uani 1 1 d .
H23A H 0.7953 0.6462 0.0222 0.131 Uiso 1 1 calc R
H23B H 0.8414 0.5578 0.0170 0.131 Uiso 1 1 calc R
H23C H 0.9009 0.6303 -0.0026 0.131 Uiso 1 1 calc R
C4 C 0.7853(9) 0.2723(6) 0.2651(3) 0.154(4) Uani 1 1 d .
H4A H 0.8507 0.2994 0.2781 0.185 Uiso 1 1 calc R
C5 C 0.7297(7) 0.2067(5) 0.2773(2) 0.124(3) Uani 1 1 d .
H5A H 0.7500 0.1809 0.3008 0.148 Uiso 1 1 calc R
C14 C 1.2861(8) 0.2975(5) 0.1140(3) 0.133(3) Uani 1 1 d .
H14A H 1.3547 0.2621 0.1203 0.159 Uiso 1 1 calc R
H14B H 1.2443 0.3024 0.1367 0.159 Uiso 1 1 calc R
C15 C 1.2113(10) 0.2651(6) 0.0851(3) 0.158(4) Uani 1 1 d .
H15A H 1.1860 0.2124 0.0925 0.237 Uiso 1 1 calc R
H15B H 1.2526 0.2604 0.0627 0.237 Uiso 1 1 calc R
H15C H 1.1422 0.2993 0.0795 0.237 Uiso 1 1 calc R
C18 C 1.4020(9) 0.5678(6) 0.1977(3) 0.148(3) Uiso 1 1 d .
H18A H 1.3672 0.5751 0.2215 0.178 Uiso 1 1 calc R
H18B H 1.4428 0.6172 0.1919 0.178 Uiso 1 1 calc R
C19 C 1.4945(13) 0.4923(9) 0.2009(4) 0.237(7) Uiso 1 1 d .
H19A H 1.5556 0.5008 0.2221 0.356 Uiso 1 1 calc R
H19B H 1.5314 0.4879 0.1776 0.356 Uiso 1 1 calc R
H19C H 1.4515 0.4433 0.2050 0.356 Uiso 1 1 calc R
C11 C 1.4727(10) 0.6876(6) -0.0038(3) 0.155(4) Uani 1 1 d .
H11A H 1.5179 0.6790 -0.0251 0.232 Uiso 1 1 calc R
H11B H 1.5206 0.7179 0.0157 0.232 Uiso 1 1 calc R
H11C H 1.4007 0.7172 -0.0123 0.232 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'
Mn Mn 0.3368 0.7283 '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 78.72(11) . .
O2 Re1 Br2 94.25(8) . .
O1 Re1 Br2 172.65(8) . .
O2 Re1 Br3 169.51(8) . .
O1 Re1 Br3 90.86(8) . .
Br2 Re1 Br3 96.21(2) . .
O2 Re1 Br4 86.63(9) . .
O1 Re1 Br4 89.01(9) . .
Br2 Re1 Br4 92.72(2) . .
Br3 Re1 Br4 92.10(2) . .
O2 Re1 Br1 88.28(10) . .
O1 Re1 Br1 86.01(9) . .
Br2 Re1 Br1 91.70(2) . .
Br3 Re1 Br1 92.18(2) . .
Br4 Re1 Br1 173.49(2) . .
N1 Mn1 n1 93.0(2) . 2_655
N1 Mn1 O4 90.00(13) . 2_655
N1 Mn1 O4 102.94(13) 2_655 2_655
N1 Mn1 O4 102.94(13) . .
N1 Mn1 O4 90.00(13) 2_655 .
O4 Mn1 O4 161.27(16) 2_655 .
N1 Mn1 O3 164.61(13) . 2_655
N1 Mn1 O3 91.39(15) 2_655 2_655
O4 Mn1 O3 74.63(10) 2_655 2_655
O4 Mn1 O3 91.80(11) . 2_655
N1 Mn1 O3 91.39(14) . .
N1 Mn1 O3 164.61(13) 2_655 .
O4 Mn1 O3 91.80(11) 2_655 .
O4 Mn1 O3 74.63(10) . .
O3 Mn1 O3 88.27(18) 2_655 .
C6 O3 Mn1 113.4(3) . .
C6 O1 Re1 114.9(3) . .
C7 O4 Mn1 114.1(3) . .
C7 O2 Re1 115.3(2) . .
C20 n2 C8 111.8(4) . .
C20 n2 C16 109.0(4) . .
C8 n2 C16 108.1(3) . .
C20 n2 C12 108.3(3) . .
C8 n2 C12 108.4(4) . .
C16 n2 C12 111.2(4) . .
C2 n1 C5 104.4(5) . .
C2 n1 Mn1 122.5(4) . .
C5 n1 Mn1 132.9(4) . .
O4 C7 O2 126.1(4) . .
O4 C7 C6 118.8(4) . .
O2 C7 C6 115.1(3) . .
O3 C6 O1 125.6(4) . .
O3 C6 C7 118.6(4) . .
O1 C6 C7 115.7(4) . .
C21 C20 n2 116.3(4) . .
C20 C21 C22 110.2(4) . .
C17 C16 n2 115.3(4) . .
C13 C12 n2 115.3(4) . .
C9 C8 n2 116.9(4) . .
C8 C9 C10 107.2(6) . .
C11 C10 C9 113.3(8) . .
C12 C13 C14 112.1(6) . .
C16 C17 C18 109.7(6) . .
C2 n3 C4 106.7(5) . .
C21 C22 C23 111.7(4) . .
N1 C2 n3 112.8(5) . .
N3 C4 C5 106.3(6) . .
N1 C5 C4 109.7(6) . .
C15 C14 C13 110.7(10) . .
C17 C18 C19 105.4(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 O2 2.081(3) .
Re1 O1 2.086(3) .
Re1 Br2 2.4471(6) .
Re1 Br3 2.4516(5) .
Re1 Br4 2.4852(5) .
Re1 Br1 2.4866(6) .
Mn1 n1 2.165(4) .
Mn1 n1 2.165(4) 2_655
Mn1 O4 2.241(3) 2_655
Mn1 O4 2.241(3) .
Mn1 O3 2.255(3) 2_655
Mn1 O3 2.255(3) .
O3 C6 1.230(5) .
O1 C6 1.274(5) .
O4 C7 1.220(5) .
O2 C7 1.278(5) .
N2 C20 1.511(5) .
N2 C8 1.518(6) .
N2 C16 1.522(6) .
N2 C12 1.529(6) .
N1 C2 1.293(6) .
N1 C5 1.337(7) .
C7 C6 1.544(5) .
C20 C21 1.509(7) .
C21 C22 1.513(7) .
C16 C17 1.505(7) .
C12 C13 1.518(8) .
C8 C9 1.475(8) .
C9 C10 1.582(9) .
C10 C11 1.354(10) .
C13 C14 1.584(11) .
C17 C18 1.546(11) .
N3 C2 1.308(7) .
N3 C4 1.325(9) .
C22 C23 1.517(7) .
C4 C5 1.345(10) .
C14 C15 1.349(12) .
C18 C19 1.617(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 2.08 2.937(6) 177.0 4_655
