#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:15:54 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179683 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/05/7000545.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_7000545
loop_
_publ_author_name
'Dorson, Frédérick'
'Molard, Yann'
'Cordier, Stéphane'
'Fabre, Bruno'
'Efremova, Olga'
'Rondeau, David'
'Mironov, Yuri'
'Cîrcu, Viorel'
'Naumov, Nikolay'
'Perrin, Christiane'
_publ_section_title
;
 Selective functionalisation of Re6 cluster anionic units: from
 hexa-hydroxo [Re6Q8(OH)6]4− (Q = S, Se) to neutral
 trans-[Re6Q8L4L′2] hybrid building blocks
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1297
_journal_paper_doi               10.1039/b822105g
_journal_year                    2009
_chemical_formula_moiety         'C36 H54 N4 O2 Re6 Se8'
_chemical_formula_sum            'C36 H54 N4 O2 Re6 Se8'
_chemical_formula_weight         2296.5
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_audit_creation_date             2007-03-09T14:41:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.340(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.7088(6)
_cell_length_b                   18.09380(5)
_cell_length_c                   9.6298(3)
_cell_measurement_reflns_used    18523
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     3075.86(14)
_computing_cell_refinement
'Dirax/lsq (DuiSenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (DuiSenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19626
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    16.519
_exptl_absorpt_correction_T_max  0.3594
_exptl_absorpt_correction_T_min  0.2306
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
[Sheldrick, G.M. (2002).SADABS version 2.03.Bruker AXS Inc., Madison,
Wisconsin, USA]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.48
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       paralelogram
_exptl_crystal_F_000             2018
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.041
_platon_squeeze_details
;
;
_refine_diff_density_max         1.51
_refine_diff_density_min         -1.395
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         3691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0322P)²+16.6431P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                2358
_reflns_number_total             3691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b822105g.txt
_cod_data_source_block           squiz
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7000545
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
Re1 Re 0.09965(3) 0 0.00153(5) 0.02342(14) Uani 1 d S . .
Re2 Re 0.02427(2) 0.072304(18) 0.14407(3) 0.02135(11) Uani 1 d . . .
Se1 Se 0.14144(8) 0 0.27931(14) 0.0300(3) Uani 1 d S . .
Se2 Se 0.04907(8) 0 -0.27636(14) 0.0282(3) Uani 1 d S . .
Se3 Se 0.09481(6) 0.13968(5) -0.00024(10) 0.0299(2) Uani 1 d . . .
O1 O 0.2136(6) 0 0.0037(10) 0.041(2) Uani 1 d S . .
N10 N 0.0560(5) 0.1579(4) 0.3157(8) 0.0308(19) Uani 1 d . . .
C1 C 0.0601(7) 0.2293(5) 0.2861(11) 0.043(3) Uani 1 d . . .
H1 H 0.0429 0.2442 0.1882 0.051 Uiso 1 calc R . .
C2 C 0.0824(7) 0.1382(6) 0.4603(10) 0.040(3) Uani 1 d . . .
H2 H 0.0808 0.0888 0.4861 0.048 Uiso 1 calc R . .
C3 C 0.1119(7) 0.1910(6) 0.5709(10) 0.043(3) Uani 1 d . . .
H3 H 0.1284 0.1756 0.6686 0.052 Uiso 1 calc R . .
C4 C 0.1174(6) 0.2638(6) 0.5415(11) 0.042(3) Uani 1 d . . .
C5 C 0.0889(7) 0.2826(6) 0.3935(12) 0.057(4) Uani 1 d . . .
H5 H 0.089 0.3319 0.366 0.069 Uiso 1 calc R . .
C6 C 0.1557(9) 0.3201(7) 0.6545(15) 0.067(4) Uani 1 d . . .
C7 C 0.2339(13) 0.3316(11) 0.6472(19) 0.157(6) Uani 1 d . . .
H7A H 0.2303 0.349 0.5509 0.236 Uiso 1 calc R . .
H7B H 0.2611 0.2857 0.6665 0.236 Uiso 1 calc R . .
H7C H 0.2602 0.3675 0.7195 0.236 Uiso 1 calc R . .
C8 C 0.1700(13) 0.2952(11) 0.803(2) 0.157(6) Uani 1 d . . .
H8A H 0.1948 0.3337 0.8702 0.236 Uiso 1 calc R . .
H8B H 0.2019 0.2523 0.8209 0.236 Uiso 1 calc R . .
H8C H 0.1229 0.283 0.8168 0.236 Uiso 1 calc R . .
C9 C 0.1092(13) 0.3879(11) 0.6410(19) 0.157(6) Uani 1 d . . .
H9A H 0.0979 0.4081 0.5439 0.236 Uiso 1 calc R . .
H9B H 0.1368 0.4236 0.7124 0.236 Uiso 1 calc R . .
H9C H 0.0628 0.3758 0.658 0.236 Uiso 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.231 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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
O1 Re1 Se2 91.9(3) . . ?
O1 Re1 Se1 91.8(3) . . ?
Se2 Re1 Se1 176.28(5) . . ?
O1 Re1 Se3 91.93(3) . 6 ?
Se2 Re1 Se3 89.59(2) . 6 ?
Se1 Re1 Se3 90.28(2) . 6 ?
O1 Re1 Se3 91.93(3) . . ?
Se2 Re1 Se3 89.59(2) . . ?
Se1 Re1 Se3 90.28(2) . . ?
Se3 Re1 Se3 176.08(5) 6 . ?
O1 Re1 Re2 134.99(18) . 6 ?
Se2 Re1 Re2 118.50(3) . 6 ?
Se1 Re1 Re2 58.45(3) . 6 ?
Se3 Re1 Re2 58.69(2) 6 6 ?
Se3 Re1 Re2 118.57(3) . 6 ?
O1 Re1 Re2 134.99(18) . . ?
Se2 Re1 Re2 118.50(3) . . ?
Se1 Re1 Re2 58.45(3) . . ?
Re2 Re1 Re2 59.899(19) 6 . ?
O1 Re1 Re2 135.27(18) . 5 ?
Se2 Re1 Re2 58.65(3) . 5 ?
Se1 Re1 Re2 118.31(4) . 5 ?
Re2 Re1 Re2 59.867(16) 6 5 ?
Re2 Re1 Re2 89.731(19) . 5 ?
O1 Re1 Re2 135.27(18) . 2 ?
Se2 Re1 Re2 58.65(3) . 2 ?
Se1 Re1 Re2 118.31(4) . 2 ?
Se3 Re1 Re2 118.09(3) 6 2 ?
Se3 Re1 Re2 58.35(2) . 2 ?
Re2 Re1 Re2 89.731(19) 6 2 ?
Re2 Re1 Re2 59.867(16) . 2 ?
Re2 Re1 Re2 59.746(18) 5 2 ?
N10 Re2 Se1 90.3(2) . . ?
N10 Re2 Se3 92.4(2) . 2 ?
Se1 Re2 Se3 177.29(3) . 2 ?
N10 Re2 Se3 90.8(2) . . ?
Se1 Re2 Se3 90.65(4) . . ?
Se3 Re2 Se3 89.54(4) 2 . ?
N10 Re2 Se2 92.4(2) . 5 ?
Se1 Re2 Se2 89.73(4) . 5 ?
Se3 Re2 Se2 89.93(4) 2 5 ?
Se3 Re2 Se2 176.78(3) . 5 ?
N10 Re2 Re2 134.79(19) . 6 ?
Se1 Re2 Re2 58.646(18) . 6 ?
Se3 Re2 Re2 119.00(2) 2 6 ?
Se3 Re2 Re2 118.87(2) . 6 ?
Se2 Re2 Re2 58.791(18) 5 6 ?
N10 Re2 Re2 135.18(19) . 2 ?
Se1 Re2 Re2 119.06(4) . 2 ?
Se3 Re2 Re2 58.88(2) 2 2 ?
Se3 Re2 Re2 58.51(2) . 2 ?
Se2 Re2 Re2 118.62(4) 5 2 ?
Re2 Re2 Re2 90 6 2 ?
N10 Re2 Re1 133.4(2) . . ?
Se1 Re2 Re1 58.90(3) . . ?
Se3 Re2 Re1 119.06(3) 2 . ?
Se3 Re2 Re1 58.84(2) . . ?
Se2 Re2 Re1 118.83(2) 5 . ?
Re2 Re2 Re1 60.050(9) 6 . ?
Re2 Re2 Re1 60.182(16) 2 . ?
N10 Re2 Re1 136.3(2) . 5 ?
Se1 Re2 Re1 118.77(2) . 5 ?
Se3 Re2 Re1 58.88(2) 2 5 ?
Se3 Re2 Re1 118.46(3) . 5 ?
Se2 Re2 Re1 58.68(3) 5 5 ?
Re2 Re2 Re1 60.127(9) 6 5 ?
Re2 Re2 Re1 59.951(16) 2 5 ?
Re1 Re2 Re1 90.269(19) . 5 ?
Re2 Se1 Re2 62.71(4) 6 . ?
Re2 Se1 Re1 62.65(3) 6 . ?
Re2 Se1 Re1 62.65(3) . . ?
Re2 Se2 Re2 62.42(4) 2 5 ?
Re2 Se2 Re1 62.67(3) 2 . ?
Re2 Se2 Re1 62.67(3) 5 . ?
Re2 Se3 Re2 62.61(3) 2 . ?
Re2 Se3 Re1 62.77(3) 2 . ?
Re2 Se3 Re1 62.47(3) . . ?
C1 N10 C2 116.5(8) . . ?
C1 N10 Re2 122.9(6) . . ?
C2 N10 Re2 120.0(6) . . ?
N10 C1 C5 123.5(9) . . ?
N10 C2 C3 121.1(9) . . ?
C4 C3 C2 122.8(9) . . ?
C3 C4 C5 114.9(9) . . ?
C3 C4 C6 124.2(11) . . ?
C5 C4 C6 120.8(11) . . ?
C1 C5 C4 121.2(10) . . ?
C8 C6 C9 104.9(15) . . ?
C8 C6 C4 113.5(12) . . ?
C9 C6 C4 112.0(13) . . ?
C8 C6 C7 103.1(15) . . ?
C9 C6 C7 115.7(14) . . ?
C4 C6 C7 107.5(12) . . ?
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
Re1 O1 2.125(10) . ?
Re1 Se2 2.5257(14) . ?
Re1 Se1 2.5262(14) . ?
Re1 Se3 2.5288(10) 6 ?
Re1 Se3 2.5288(10) . ?
Re1 Re2 2.6205(6) 6 ?
Re1 Re2 2.6205(6) . ?
Re1 Re2 2.6266(5) 5 ?
Re1 Re2 2.6266(5) 2 ?
Re2 N10 2.198(7) . ?
Re2 Se1 2.5143(13) . ?
Re2 Se3 2.5147(10) 2 ?
Re2 Se3 2.5246(10) . ?
Re2 Se2 2.5248(13) 5 ?
Re2 Re2 2.6165(6) 6 ?
Re2 Re2 2.6183(6) 2 ?
Re2 Re1 2.6266(5) 5 ?
Se1 Re2 2.5143(13) 6 ?
Se2 Re2 2.5248(13) 2 ?
Se2 Re2 2.5248(13) 5 ?
Se3 Re2 2.5147(10) 2 ?
N10 C1 1.331(11) . ?
N10 C2 1.362(11) . ?
C1 C5 1.387(13) . ?
C2 C3 1.401(13) . ?
C3 C4 1.359(14) . ?
C4 C5 1.388(14) . ?
C4 C6 1.489(13) . ?
C6 C8 1.44(2) . ?
C6 C9 1.48(2) . ?
C6 C7 1.50(2) . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.000 445 149 ' '
2 0.000 0.500 0.000 445 149 ' '
