#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/54/4325424.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_4325424
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 Co O8 Re2 n6'
_chemical_formula_weight         1867.73
_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                 96.082(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2017(13)
_cell_length_b                   16.4144(13)
_cell_length_c                   34.732(4)
_cell_measurement_temperature    293(2)
_cell_volume                     6350.2(12)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            44935
_diffrn_reflns_theta_full        28.74
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    9.141
_exptl_absorpt_correction_T_max  0.393
_exptl_absorpt_correction_T_min  0.332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             3580
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.289
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         8236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0363
_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)+(0.0374P)²+22.0405P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                6482
_reflns_number_total             8236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200531s_si_003.cif
_cod_data_source_block           Compound2_re2co
_cod_original_cell_volume        6350.1(11)
_cod_original_formula_sum        'C42 H80 Br8 Co n6 O8 Re2'
_cod_database_code               4325424
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 0.687375(16) -0.098677(11) 0.372022(5) 0.04769(7) Uani 1 1 d .
Co1 Co 0.5000 0.09280(5) 0.2500 0.04394(18) Uani 1 2 d S
Br3 Br 0.85244(5) -0.19741(4) 0.376994(19) 0.07263(17) Uani 1 1 d .
Br2 Br 0.63162(6) -0.11976(4) 0.437633(17) 0.07632(18) Uani 1 1 d .
Br4 Br 0.82527(5) 0.01508(4) 0.39297(2) 0.07929(18) Uani 1 1 d .
Br1 Br 0.53975(6) -0.20262(5) 0.34542(2) 0.0878(2) Uani 1 1 d .
O3 O 0.6310(3) -0.0030(2) 0.26347(9) 0.0549(8) Uani 1 1 d .
O1 O 0.7126(3) -0.0732(2) 0.31460(9) 0.0544(8) Uani 1 1 d .
O4 O 0.4912(3) 0.07531(19) 0.31062(9) 0.0509(7) Uani 1 1 d .
O2 O 0.5576(3) -0.0100(2) 0.35830(9) 0.0546(8) Uani 1 1 d .
N2 n 1.2644(3) 0.5323(3) 0.09226(12) 0.0560(10) Uani 1 1 d .
N1 n 0.6345(4) 0.1788(3) 0.25303(12) 0.0570(10) Uani 1 1 d .
C7 C 0.5548(4) 0.0194(3) 0.32393(12) 0.0446(9) Uani 1 1 d .
C6 C 0.6393(4) -0.0218(3) 0.29764(13) 0.0447(9) Uani 1 1 d .
C20 C 1.1525(4) 0.5842(3) 0.08940(15) 0.0549(11) Uani 1 1 d .
H20A H 1.1767 0.6409 0.0912 0.066 Uiso 1 1 calc R
H20B H 1.1096 0.5725 0.1116 0.066 Uiso 1 1 calc R
C21 C 1.0656(5) 0.5731(4) 0.05257(17) 0.0651(14) Uani 1 1 d .
H21A H 1.1041 0.5902 0.0302 0.078 Uiso 1 1 calc R
H21B H 1.0440 0.5161 0.0494 0.078 Uiso 1 1 calc R
C16 C 1.3460(5) 0.5588(4) 0.12742(16) 0.0700(15) Uani 1 1 d .
H16A H 1.3622 0.6165 0.1250 0.084 Uiso 1 1 calc R
H16B H 1.4218 0.5303 0.1274 0.084 Uiso 1 1 calc R
C12 C 1.2273(5) 0.4432(3) 0.0953(2) 0.0712(15) Uani 1 1 d .
H12A H 1.1768 0.4382 0.1162 0.085 Uiso 1 1 calc R
H12B H 1.1792 0.4281 0.0714 0.085 Uiso 1 1 calc R
C8 C 1.3332(5) 0.5413(4) 0.05712(17) 0.0762(17) Uani 1 1 d .
H8A H 1.4068 0.5100 0.0618 0.091 Uiso 1 1 calc R
H8B H 1.2858 0.5167 0.0351 0.091 Uiso 1 1 calc R
C9 C 1.3651(7) 0.6249(5) 0.0462(2) 0.096(2) Uani 1 1 d .
H9A H 1.4118 0.6516 0.0677 0.115 Uiso 1 1 calc R
H9B H 1.2931 0.6566 0.0391 0.115 Uiso 1 1 calc R
C10 C 1.4403(9) 0.6173(6) 0.0110(3) 0.129(3) Uani 1 1 d .
H10A H 1.5132 0.5874 0.0193 0.154 Uiso 1 1 calc R
H10B H 1.3948 0.5851 -0.0089 0.154 Uiso 1 1 calc R
C13 C 1.3300(6) 0.3836(4) 0.1023(3) 0.106(3) Uani 1 1 d .
H13A H 1.3870 0.4040 0.1231 0.127 Uiso 1 1 calc R
H13B H 1.3710 0.3796 0.0792 0.127 Uiso 1 1 calc R
C17 C 1.2988(6) 0.5444(5) 0.16600(19) 0.095(2) Uani 1 1 d .
H17A H 1.2767 0.4876 0.1681 0.114 Uiso 1 1 calc R
H17B H 1.2275 0.5772 0.1677 0.114 Uiso 1 1 calc R
N3 n 0.7284(6) 0.2863(4) 0.2345(2) 0.113(2) Uani 1 1 d .
H3A H 0.7447 0.3270 0.2203 0.135 Uiso 1 1 calc R
C22 C 0.9544(5) 0.6235(4) 0.05564(17) 0.0695(15) Uani 1 1 d .
H22A H 0.9767 0.6804 0.0590 0.083 Uiso 1 1 calc R
H22B H 0.9168 0.6064 0.0782 0.083 Uiso 1 1 calc R
C2 C 0.6417(7) 0.2317(5) 0.2256(2) 0.092(2) Uani 1 1 d .
H2A H 0.5921 0.2315 0.2023 0.111 Uiso 1 1 calc R
C23 C 0.8651(6) 0.6142(4) 0.0195(2) 0.092(2) Uani 1 1 d .
H23A H 0.7955 0.6470 0.0221 0.137 Uiso 1 1 calc R
H23B H 0.8417 0.5581 0.0165 0.137 Uiso 1 1 calc R
H23C H 0.9020 0.6316 -0.0028 0.137 Uiso 1 1 calc R
C4 C 0.7828(10) 0.2683(7) 0.2674(3) 0.162(5) Uani 1 1 d .
H4A H 0.8499 0.2934 0.2803 0.195 Uiso 1 1 calc R
C5 C 0.7188(9) 0.2023(6) 0.2795(3) 0.141(4) Uani 1 1 d .
H5A H 0.7342 0.1779 0.3037 0.169 Uiso 1 1 calc R
C14 C 1.2864(8) 0.2964(6) 0.1134(4) 0.143(4) Uani 1 1 d .
H14A H 1.3556 0.2609 0.1182 0.172 Uiso 1 1 calc R
H14B H 1.2485 0.3002 0.1372 0.172 Uiso 1 1 calc R
C15 C 1.2099(11) 0.2639(7) 0.0862(4) 0.167(5) Uani 1 1 d .
H15A H 1.1859 0.2111 0.0944 0.251 Uiso 1 1 calc R
H15B H 1.2476 0.2587 0.0628 0.251 Uiso 1 1 calc R
H15C H 1.1405 0.2984 0.0816 0.251 Uiso 1 1 calc R
C18 C 1.3931(11) 0.5664(8) 0.1989(4) 0.160(4) Uiso 1 1 d .
H18A H 1.3573 0.5741 0.2229 0.192 Uiso 1 1 calc R
H18B H 1.4357 0.6156 0.1931 0.192 Uiso 1 1 calc R
C19 C 1.4825(15) 0.4874(11) 0.2016(5) 0.254(8) Uiso 1 1 d .
H19A H 1.5443 0.4947 0.2227 0.381 Uiso 1 1 calc R
H19B H 1.5184 0.4820 0.1778 0.381 Uiso 1 1 calc R
H19C H 1.4373 0.4391 0.2059 0.381 Uiso 1 1 calc R
C11 C 1.4708(11) 0.6868(8) -0.0049(4) 0.177(5) Uani 1 1 d .
H11A H 1.5160 0.6754 -0.0262 0.266 Uiso 1 1 calc R
H11B H 1.5188 0.7186 0.0141 0.266 Uiso 1 1 calc R
H11C H 1.3996 0.7166 -0.0140 0.266 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'
Co Co 0.3494 0.9721 '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 94.08(8) . .
O1 Re1 Br2 172.36(9) . .
O2 Re1 Br3 169.79(8) . .
O1 Re1 Br3 91.28(8) . .
Br2 Re1 Br3 96.07(2) . .
O2 Re1 Br4 86.49(10) . .
O1 Re1 Br4 89.21(10) . .
Br2 Re1 Br4 92.62(3) . .
Br3 Re1 Br4 92.03(2) . .
O2 Re1 Br1 88.50(10) . .
O1 Re1 Br1 86.24(10) . .
Br2 Re1 Br1 91.36(3) . .
Br3 Re1 Br1 92.27(3) . .
Br4 Re1 Br1 173.81(3) . .
N1 Co1 n1 93.5(3) . 2_655
N1 Co1 O4 91.86(14) . 2_655
N1 Co1 O4 98.72(15) 2_655 2_655
N1 Co1 O4 98.72(15) . .
N1 Co1 O4 91.86(14) 2_655 .
O4 Co1 O4 164.57(18) 2_655 .
N1 Co1 O3 169.46(14) . 2_655
N1 Co1 O3 90.65(16) 2_655 2_655
O4 Co1 O3 77.92(11) 2_655 2_655
O4 Co1 O3 90.83(12) . 2_655
N1 Co1 O3 90.65(16) . .
N1 Co1 O3 169.46(14) 2_655 .
O4 Co1 O3 90.83(12) 2_655 .
O4 Co1 O3 77.92(11) . .
O3 Co1 O3 86.98(19) 2_655 .
C6 O3 Co1 111.9(3) . .
C6 O1 Re1 115.3(3) . .
C7 O4 Co1 112.8(3) . .
C7 O2 Re1 115.1(3) . .
C20 n2 C16 108.5(4) . .
C20 n2 C8 112.4(4) . .
C16 n2 C8 107.8(4) . .
C20 n2 C12 108.4(4) . .
C16 n2 C12 111.5(5) . .
C8 n2 C12 108.2(4) . .
C2 n1 C5 102.9(6) . .
C2 n1 Co1 121.5(4) . .
C5 n1 Co1 135.2(5) . .
O4 C7 O2 126.1(4) . .
O4 C7 C6 118.4(4) . .
O2 C7 C6 115.4(4) . .
O3 C6 O1 126.5(4) . .
O3 C6 C7 118.5(4) . .
O1 C6 C7 115.0(4) . .
N2 C20 C21 115.9(4) . .
C22 C21 C20 109.4(4) . .
N2 C16 C17 115.7(5) . .
C13 C12 n2 115.0(5) . .
C9 C8 n2 117.0(5) . .
C8 C9 C10 107.0(7) . .
C11 C10 C9 116.1(10) . .
C12 C13 C14 112.2(6) . .
C16 C17 C18 110.5(7) . .
C4 n3 C2 108.7(7) . .
C21 C22 C23 111.1(5) . .
N1 C2 n3 112.3(6) . .
N1 C2 C5 38.7(4) . .
N3 C2 C5 73.6(5) . .
N3 C4 C5 103.9(8) . .
N1 C5 C4 112.0(8) . .
N1 C5 C2 38.4(4) . .
C4 C5 C2 73.6(6) . .
C15 C14 C13 112.7(11) . .
C17 C18 C19 103.2(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 O2 2.077(3) .
Re1 O1 2.086(3) .
Re1 Br2 2.4503(6) .
Re1 Br3 2.4511(6) .
Re1 Br4 2.4827(6) .
Re1 Br1 2.4850(7) .
Co1 n1 2.059(4) .
Co1 n1 2.059(4) 2_655
Co1 O4 2.138(3) 2_655
Co1 O4 2.138(3) .
Co1 O3 2.168(3) 2_655
Co1 O3 2.168(3) .
O3 C6 1.220(5) .
O1 C6 1.277(5) .
O4 C7 1.221(5) .
O2 C7 1.285(5) .
N2 C20 1.510(6) .
N2 C16 1.510(7) .
N2 C8 1.518(6) .
N2 C12 1.526(7) .
N1 C2 1.298(8) .
N1 C5 1.306(9) .
C7 C6 1.540(6) .
C20 C21 1.534(7) .
C21 C22 1.508(7) .
C16 C17 1.510(8) .
C12 C13 1.511(8) .
C8 C9 1.478(10) .
C9 C10 1.562(10) .
C10 C11 1.326(12) .
C13 C14 1.573(13) .
C17 C18 1.515(13) .
N3 C4 1.271(11) .
N3 C2 1.334(8) .
C22 C23 1.528(8) .
C2 C5 2.036(11) .
C4 C5 1.389(12) .
C14 C15 1.320(14) .
C18 C19 1.635(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 2.12 2.984(7) 179.2 4_655
