#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:09:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179096 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/58/4305884.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_4305884
loop_
_publ_author_name
'Pabitra Baran Chatterjee'
'Sk Md Towsif Abtab'
'Kisholoy Bhattacharya'
'Akira Endo'
'Elizabeth J. Shotton'
'Simon J. Teat'
'Muktimoy Chaudhury'
_publ_section_title
;
Hetero-Bimetallic Complexes Involving Vanadium(V) and Rhenium(VII) Centers,
Connected by Unsupported μ-Oxido Bridge: Synthesis, Characterization, and
Redox Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8830
_journal_page_last               8838
_journal_paper_doi               10.1021/ic800815p
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C18 H20 N2 O10 Re V'
_chemical_formula_weight         661.50
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.625(2)
_cell_angle_beta                 85.627(2)
_cell_angle_gamma                64.734(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2522(7)
_cell_length_b                   9.1776(8)
_cell_length_c                   15.1526(13)
_cell_measurement_reflns_used    5570
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.13
_cell_measurement_theta_min      4.18
_cell_volume                     1034.35(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with wide frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 16.2'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8460
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7434
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         4.28
_exptl_absorpt_coefficient_mu    9.905
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2004/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.005
_refine_diff_density_max         4.112
_refine_diff_density_min         -4.414
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4163
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0431
_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)+(0.0807P)²+1.8601P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                3973
_reflns_number_total             4163
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic800815p_si_002_1.cif
_cod_data_source_block           MC1
_cod_database_code               4305884
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
V1 V 0.21116(12) 0.59561(10) 0.24070(6) 0.0111(2) Uani 1 1 d . . .
C1 C 0.5817(7) 0.3523(6) 0.2152(4) 0.0135(11) Uani 1 1 d . . .
O1 O 0.4177(5) 0.4407(5) 0.1883(3) 0.0147(8) Uani 1 1 d . . .
C2 C 0.6954(8) 0.2084(7) 0.1647(4) 0.0166(11) Uani 1 1 d . . .
O2 O 0.6155(5) 0.1748(5) 0.0968(3) 0.0192(9) Uani 1 1 d . . .
C3 C 0.8675(8) 0.1202(7) 0.1880(4) 0.0222(13) Uani 1 1 d . . .
H3 H 0.9438 0.0239 0.1556 0.027 Uiso 1 1 calc R . .
C4 C 0.9311(8) 0.1709(8) 0.2587(5) 0.0238(13) Uani 1 1 d . . .
H4 H 1.0507 0.1085 0.2734 0.029 Uiso 1 1 calc R . .
C5 C 0.8250(8) 0.3087(8) 0.3074(4) 0.0224(13) Uani 1 1 d . . .
H5 H 0.8707 0.3414 0.3554 0.027 Uiso 1 1 calc R . .
C6 C 0.6473(7) 0.4014(7) 0.2855(4) 0.0149(11) Uani 1 1 d . . .
C7 C 0.5408(8) 0.5480(7) 0.3350(4) 0.0160(11) Uani 1 1 d U . .
H7 H 0.5968 0.5794 0.3789 0.019 Uiso 1 1 calc R . .
N1 N 0.3745(6) 0.6409(6) 0.3247(3) 0.0149(9) Uani 1 1 d U . .
C8 C 0.2803(8) 0.7869(7) 0.3802(4) 0.0217(12) Uani 1 1 d U . .
H8A H 0.2596 0.8838 0.3451 0.026 Uiso 1 1 calc R . .
H8B H 0.3518 0.7861 0.4300 0.026 Uiso 1 1 calc R . .
C9 C 0.1025(8) 0.7873(8) 0.4147(4) 0.0221(13) Uani 1 1 d U . .
H9A H 0.1216 0.7049 0.4603 0.027 Uiso 1 1 calc R . .
H9B H 0.0201 0.8941 0.4413 0.027 Uiso 1 1 calc R . .
N2 N 0.0267(7) 0.7499(6) 0.3375(3) 0.0149(9) Uani 1 1 d U . .
C10 C -0.1417(8) 0.8234(7) 0.3283(4) 0.0174(12) Uani 1 1 d U . .
H10 H -0.2143 0.9058 0.3705 0.021 Uiso 1 1 calc R . .
C11 C -0.2284(8) 0.7878(7) 0.2566(4) 0.0176(11) Uani 1 1 d . . .
C12 C -0.4097(8) 0.8910(7) 0.2442(4) 0.0209(12) Uani 1 1 d . . .
H12 H -0.4724 0.9844 0.2813 0.025 Uiso 1 1 calc R . .
C13 C -0.4950(8) 0.8565(7) 0.1789(4) 0.0215(12) Uani 1 1 d . . .
H13 H -0.6162 0.9277 0.1707 0.026 Uiso 1 1 calc R . .
C14 C -0.4072(8) 0.7189(7) 0.1242(4) 0.0190(12) Uani 1 1 d . . .
H14 H -0.4683 0.6975 0.0790 0.023 Uiso 1 1 calc R . .
C15 C -0.2293(8) 0.6127(7) 0.1361(4) 0.0156(11) Uani 1 1 d . . .
O4 O -0.1303(6) 0.4743(5) 0.0883(3) 0.0196(9) Uani 1 1 d . . .
C16 C -0.1381(7) 0.6481(7) 0.2014(4) 0.0147(11) Uani 1 1 d . . .
O3 O 0.0302(5) 0.5431(5) 0.2129(3) 0.0151(8) Uani 1 1 d . . .
C17 C 0.7261(8) 0.0379(7) 0.0416(4) 0.0230(13) Uani 1 1 d U . .
H17A H 0.8266 0.0549 0.0125 0.035 Uiso 1 1 calc R . .
H17B H 0.6549 0.0226 -0.0033 0.035 Uiso 1 1 calc R . .
H17C H 0.7730 -0.0581 0.0778 0.035 Uiso 1 1 calc R . .
C18 C -0.2066(9) 0.4410(8) 0.0140(4) 0.0244(13) Uani 1 1 d . . .
H18A H -0.3159 0.4292 0.0342 0.037 Uiso 1 1 calc R . .
H18B H -0.1197 0.3409 -0.0162 0.037 Uiso 1 1 calc R . .
H18C H -0.2366 0.5300 -0.0271 0.037 Uiso 1 1 calc R . .
O5 O 0.1749(5) 0.7419(5) 0.1760(3) 0.0150(8) Uani 1 1 d . . .
Re1 Re 0.29328(3) 0.27873(2) 0.430786(13) 0.01440(11) Uani 1 1 d . . .
O11 O 0.2445(6) 0.4097(5) 0.3433(3) 0.0222(9) Uani 1 1 d . . .
O12 O 0.5237(6) 0.1660(6) 0.4304(3) 0.0327(11) Uani 1 1 d . . .
O13 O 0.2174(7) 0.3864(6) 0.5283(3) 0.0287(10) Uani 1 1 d . . .
O14 O 0.1911(7) 0.1513(5) 0.4222(3) 0.0274(10) Uani 1 1 d . . .
O1W O 0.2343(8) 0.2097(6) 0.1107(5) 0.0467(14) Uani 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 -0.0020 0.0024 '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 -0.0031 0.0049 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0042 0.0089 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.2394 0.7367 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -2.7272 9.6059 '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
O5 V1 O1 101.75(19) . . ?
O5 V1 O3 99.07(19) . . ?
O1 V1 O3 106.21(18) . . ?
O5 V1 N2 90.89(19) . . ?
O1 V1 N2 160.44(19) . . ?
O3 V1 N2 86.15(19) . . ?
O5 V1 N1 98.6(2) . . ?
O1 V1 N1 86.20(18) . . ?
O3 V1 N1 155.77(19) . . ?
N2 V1 N1 77.11(19) . . ?
O5 V1 O11 173.81(19) . . ?
O1 V1 O11 83.90(17) . . ?
O3 V1 O11 81.57(17) . . ?
N2 V1 O11 83.00(18) . . ?
N1 V1 O11 79.14(17) . . ?
O1 C1 C6 122.3(5) . . ?
O1 C1 C2 117.6(5) . . ?
C6 C1 C2 119.9(5) . . ?
C1 O1 V1 134.2(4) . . ?
O2 C2 C3 127.1(5) . . ?
O2 C2 C1 114.1(5) . . ?
C3 C2 C1 118.8(6) . . ?
C2 O2 C17 116.2(5) . . ?
C2 C3 C4 120.6(6) . . ?
C5 C4 C3 121.5(6) . . ?
C4 C5 C6 119.3(6) . . ?
C1 C6 C5 119.9(5) . . ?
C1 C6 C7 121.6(5) . . ?
C5 C6 C7 118.5(5) . . ?
N1 C7 C6 125.1(5) . . ?
C7 N1 C8 119.7(5) . . ?
C7 N1 V1 126.2(4) . . ?
C8 N1 V1 114.0(4) . . ?
N1 C8 C9 106.3(5) . . ?
N2 C9 C8 106.1(5) . . ?
C10 N2 C9 120.3(5) . . ?
C10 N2 V1 123.1(4) . . ?
C9 N2 V1 116.2(4) . . ?
N2 C10 C11 123.7(6) . . ?
C16 C11 C12 119.0(6) . . ?
C16 C11 C10 121.5(5) . . ?
C12 C11 C10 119.4(5) . . ?
C13 C12 C11 120.2(6) . . ?
C12 C13 C14 121.2(5) . . ?
C13 C14 C15 120.0(6) . . ?
O4 C15 C14 125.6(5) . . ?
O4 C15 C16 114.7(5) . . ?
C14 C15 C16 119.6(5) . . ?
C15 O4 C18 117.7(5) . . ?
O3 C16 C15 118.5(5) . . ?
O3 C16 C11 121.4(5) . . ?
C15 C16 C11 119.9(5) . . ?
C16 O3 V1 125.4(4) . . ?
O13 Re1 O14 109.2(2) . . ?
O13 Re1 O12 108.5(2) . . ?
O14 Re1 O12 109.3(2) . . ?
O13 Re1 O11 109.6(2) . . ?
O14 Re1 O11 110.1(2) . . ?
O12 Re1 O11 110.0(2) . . ?
Re1 O11 V1 170.2(3) . . ?
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
V1 O5 1.593(4) . ?
V1 O1 1.816(4) . ?
V1 O3 1.831(4) . ?
V1 N2 2.079(5) . ?
V1 N1 2.087(5) . ?
V1 O11 2.243(4) . ?
C1 O1 1.341(7) . ?
C1 C6 1.390(8) . ?
C1 C2 1.434(8) . ?
C2 O2 1.367(7) . ?
C2 C3 1.374(8) . ?
O2 C17 1.425(7) . ?
C3 C4 1.392(9) . ?
C4 C5 1.371(9) . ?
C5 C6 1.410(8) . ?
C6 C7 1.431(8) . ?
C7 N1 1.291(7) . ?
N1 C8 1.461(7) . ?
C8 C9 1.519(9) . ?
C9 N2 1.475(7) . ?
N2 C10 1.278(8) . ?
C10 C11 1.456(9) . ?
C11 C16 1.415(8) . ?
C11 C12 1.415(8) . ?
C12 C13 1.370(9) . ?
C13 C14 1.395(9) . ?
C14 C15 1.398(8) . ?
C15 O4 1.357(7) . ?
C15 C16 1.407(8) . ?
O4 C18 1.427(7) . ?
C16 O3 1.334(7) . ?
Re1 O13 1.703(5) . ?
Re1 O14 1.720(4) . ?
Re1 O12 1.733(4) . ?
Re1 O11 1.736(4) . ?
