#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:26:39 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178812 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/66/4106640.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_4106640
loop_
_publ_author_name
'Richard D. Adams'
'William C. Pearl'
'Yuen Onn Wong'
'Qiang Zhang'
'Michael B. Hall'
'Justin R. Walensky'
_publ_section_title
;
 Tetrarhena-heterocycle from the Palladium-Catalyzed Dimerization of
 Re2(CO)8(μ-SbPh2)(μ-H) Exhibits an Unusual Host-Guest Behavior
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12994
_journal_page_last               12997
_journal_paper_doi               10.1021/ja205515u
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C40 H22 O16 Re4 Sb2'
_chemical_formula_weight         1746.88
_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                 118.476(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9667(18)
_cell_length_b                   13.5280(12)
_cell_length_c                   19.2161(17)
_cell_measurement_reflns_used    6042
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      2.32
_cell_volume                     4562.5(7)
_computing_cell_refinement       'SAINT+  V6.45 (Bruker, 2003)'
_computing_data_collection       'SMART V5.632 (Bruker, 2005)'
_computing_data_reduction        'SAINT+  V6.45'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27832
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    11.804
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            L-Yellow
_exptl_crystal_density_diffrn    2.543
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0247
_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)+(0.0226P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0493
_reflns_number_gt                3414
_reflns_number_total             4030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205515u_si_002_1.cif
_cod_data_source_block           5
_cod_database_code               4106640
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 0.138122(13) 0.179229(17) 0.271762(14) 0.04781(8) Uani 1 1 d .
Re2 Re 0.084586(12) -0.034004(16) 0.183051(13) 0.04357(7) Uani 1 1 d .
Sb1 Sb 0.0000 -0.11625(4) 0.2500 0.04159(13) Uani 1 2 d S
Sb2 Sb 0.0000 0.25886(4) 0.2500 0.04574(14) Uani 1 2 d S
H1 H 0.072(3) 0.058(3) 0.232(3) 0.055 Uiso 1 1 d .
C11 C 0.2347(4) 0.1348(5) 0.2827(4) 0.0645(17) Uani 1 1 d .
C12 C 0.1684(4) 0.1215(6) 0.3784(5) 0.073(2) Uani 1 1 d .
C13 C 0.1827(4) 0.3050(6) 0.3155(5) 0.078(2) Uani 1 1 d .
C14 C 0.1072(4) 0.2286(5) 0.1626(4) 0.0627(17) Uani 1 1 d .
C21 C 0.1778(4) -0.0855(5) 0.2758(4) 0.0647(17) Uani 1 1 d .
C22 C 0.0717(4) -0.1570(5) 0.1279(4) 0.0582(16) Uani 1 1 d .
C23 C 0.1430(3) 0.0170(4) 0.1334(4) 0.0509(14) Uani 1 1 d .
C24 C -0.0061(4) 0.0260(4) 0.0952(4) 0.0556(15) Uani 1 1 d .
C25 C 0.0767(3) -0.2210(4) 0.3334(3) 0.0451(13) Uani 1 1 d .
C26 C 0.0984(3) -0.3031(4) 0.3039(4) 0.0548(15) Uani 1 1 d .
H26 H 0.0780 -0.3121 0.2495 0.066 Uiso 1 1 calc R
C27 C 0.1500(4) -0.3704(5) 0.3559(4) 0.0665(18) Uani 1 1 d .
H27 H 0.1644 -0.4245 0.3362 0.080 Uiso 1 1 calc R
C28 C 0.1803(3) -0.3586(5) 0.4363(5) 0.070(2) Uani 1 1 d .
H28 H 0.2152 -0.4039 0.4711 0.084 Uiso 1 1 calc R
C29 C 0.1583(4) -0.2793(5) 0.4641(4) 0.0676(18) Uani 1 1 d .
H29 H 0.1778 -0.2715 0.5185 0.081 Uiso 1 1 calc R
C30 C 0.1077(3) -0.2104(5) 0.4138(4) 0.0569(16) Uani 1 1 d .
H30 H 0.0945 -0.1562 0.4344 0.068 Uiso 1 1 calc R
C31 C 0.0290(3) 0.3626(4) 0.3451(4) 0.0532(15) Uani 1 1 d .
C32 C 0.0849(4) 0.3403(5) 0.4194(4) 0.0697(18) Uani 1 1 d .
H32 H 0.1121 0.2816 0.4286 0.084 Uiso 1 1 calc R
C33 C 0.1013(4) 0.4059(7) 0.4816(4) 0.085(2) Uani 1 1 d .
H33 H 0.1390 0.3903 0.5325 0.101 Uiso 1 1 calc R
C34 C 0.0625(6) 0.4922(7) 0.4682(5) 0.093(3) Uani 1 1 d .
H34 H 0.0739 0.5360 0.5096 0.111 Uiso 1 1 calc R
C35 C 0.0069(6) 0.5146(6) 0.3938(6) 0.094(3) Uani 1 1 d .
H35 H -0.0196 0.5739 0.3849 0.113 Uiso 1 1 calc R
C36 C -0.0107(4) 0.4510(5) 0.3319(4) 0.0689(19) Uani 1 1 d .
H36 H -0.0489 0.4670 0.2813 0.083 Uiso 1 1 calc R
O11 O 0.2934(3) 0.1119(4) 0.2910(3) 0.0889(16) Uani 1 1 d .
O12 O 0.1895(3) 0.0885(5) 0.4389(3) 0.116(2) Uani 1 1 d .
O13 O 0.2102(3) 0.3797(4) 0.3431(4) 0.117(2) Uani 1 1 d .
O14 O 0.0901(3) 0.2571(4) 0.1014(3) 0.0927(17) Uani 1 1 d .
O21 O 0.2323(3) -0.1137(4) 0.3282(3) 0.1010(18) Uani 1 1 d .
O22 O 0.0651(3) -0.2299(3) 0.0952(3) 0.0833(15) Uani 1 1 d .
O23 O 0.1752(2) 0.0456(3) 0.1020(3) 0.0695(12) Uani 1 1 d .
O24 O -0.0552(3) 0.0661(4) 0.0439(3) 0.0813(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 0.0033 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'
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
C13 Re1 C11 89.9(3) . .
C13 Re1 C14 90.6(3) . .
C11 Re1 C14 90.6(3) . .
C13 Re1 C12 92.7(3) . .
C11 Re1 C12 88.2(3) . .
C14 Re1 C12 176.5(3) . .
C13 Re1 Sb2 86.7(2) . .
C11 Re1 Sb2 174.95(19) . .
C14 Re1 Sb2 85.72(17) . .
C12 Re1 Sb2 95.65(18) . .
C13 Re1 Re2 169.0(2) . .
C11 Re1 Re2 80.97(19) . .
C14 Re1 Re2 83.50(19) . .
C12 Re1 Re2 93.1(2) . .
Sb2 Re1 Re2 102.018(12) . .
C13 Re1 H1 166.2(14) . .
C11 Re1 H1 103.3(14) . .
C14 Re1 H1 93.3(14) . .
C12 Re1 H1 83.8(14) . .
Sb2 Re1 H1 80.4(13) . .
Re2 Re1 H1 24.5(14) . .
C22 Re2 C23 89.5(2) . .
C22 Re2 C24 93.3(3) . .
C23 Re2 C24 87.4(2) . .
C22 Re2 C21 90.7(3) . .
C23 Re2 C21 92.3(2) . .
C24 Re2 C21 176.0(3) . .
C22 Re2 Sb1 87.58(17) . .
C23 Re2 Sb1 177.04(17) . .
C24 Re2 Sb1 92.74(17) . .
C21 Re2 Sb1 87.72(18) . .
C22 Re2 Re1 167.95(17) . .
C23 Re2 Re1 79.60(17) . .
C24 Re2 Re1 91.25(17) . .
C21 Re2 Re1 84.73(19) . .
Sb1 Re2 Re1 103.347(12) . .
C22 Re2 H1 161.5(16) . .
C23 Re2 H1 107.8(17) . .
C24 Re2 H1 81.3(17) . .
C21 Re2 H1 95.0(17) . .
Sb1 Re2 H1 75.1(16) . .
Re1 Re2 H1 30.5(16) . .
C25 Sb1 C25 97.1(3) . 2
C25 Sb1 Re2 106.99(14) . 2
C25 Sb1 Re2 103.57(13) 2 2
C25 Sb1 Re2 103.57(13) . .
C25 Sb1 Re2 106.99(14) 2 .
Re2 Sb1 Re2 133.10(2) 2 .
C31 Sb2 C31 98.6(3) 2 .
C31 Sb2 Re1 106.09(16) 2 2
C31 Sb2 Re1 102.97(14) . 2
C31 Sb2 Re1 102.97(14) 2 .
C31 Sb2 Re1 106.09(16) . .
Re1 Sb2 Re1 134.75(2) 2 .
O11 C11 Re1 177.1(6) . .
O12 C12 Re1 176.0(6) . .
O13 C13 Re1 178.7(8) . .
O14 C14 Re1 179.5(8) . .
O21 C21 Re2 178.1(6) . .
O22 C22 Re2 179.0(5) . .
O23 C23 Re2 177.7(5) . .
O24 C24 Re2 174.8(5) . .
C30 C25 C26 118.5(5) . .
C30 C25 Sb1 123.5(4) . .
C26 C25 Sb1 117.9(4) . .
C27 C26 C25 119.7(6) . .
C27 C26 H26 120.2 . .
C25 C26 H26 120.2 . .
C28 C27 C26 120.9(6) . .
C28 C27 H27 119.6 . .
C26 C27 H27 119.6 . .
C29 C28 C27 118.8(6) . .
C29 C28 H28 120.6 . .
C27 C28 H28 120.6 . .
C28 C29 C30 121.5(6) . .
C28 C29 H29 119.2 . .
C30 C29 H29 119.2 . .
C25 C30 C29 120.5(6) . .
C25 C30 H30 119.7 . .
C29 C30 H30 119.7 . .
C32 C31 C36 119.6(6) . .
C32 C31 Sb2 120.0(5) . .
C36 C31 Sb2 120.5(5) . .
C31 C32 C33 119.8(7) . .
C31 C32 H32 120.1 . .
C33 C32 H32 120.1 . .
C34 C33 C32 120.3(8) . .
C34 C33 H33 119.9 . .
C32 C33 H33 119.9 . .
C33 C34 C35 119.9(8) . .
C33 C34 H34 120.1 . .
C35 C34 H34 120.1 . .
C34 C35 C36 121.0(8) . .
C34 C35 H35 119.5 . .
C36 C35 H35 119.5 . .
C35 C36 C31 119.6(7) . .
C35 C36 H36 120.2 . .
C31 C36 H36 120.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C13 1.918(7) .
Re1 C11 1.933(7) .
Re1 C14 1.998(7) .
Re1 C12 1.999(8) .
Re1 Sb2 2.8002(4) .
Re1 Re2 3.2607(4) .
Re1 H1 2.02(5) .
Re2 C22 1.923(7) .
Re2 C23 1.951(6) .
Re2 C24 1.968(7) .
Re2 C21 1.991(7) .
Re2 Sb1 2.7959(3) .
Re2 H1 1.65(5) .
Sb1 C25 2.141(5) .
Sb1 C25 2.141(5) 2
Sb1 Re2 2.7959(3) 2
Sb2 C31 2.153(6) 2
Sb2 C31 2.153(6) .
Sb2 Re1 2.8002(4) 2
C11 O11 1.147(7) .
C12 O12 1.122(7) .
C13 O13 1.151(7) .
C14 O14 1.125(7) .
C21 O21 1.140(7) .
C22 O22 1.143(7) .
C23 O23 1.138(6) .
C24 O24 1.143(7) .
C25 C30 1.369(8) .
C25 C26 1.407(7) .
C26 C27 1.382(8) .
C26 H26 0.9300 .
C27 C28 1.374(9) .
C27 H27 0.9300 .
C28 C29 1.362(9) .
C28 H28 0.9300 .
C29 C30 1.376(8) .
C29 H29 0.9300 .
C30 H30 0.9300 .
C31 C32 1.363(8) .
C31 C36 1.390(8) .
C32 C33 1.397(9) .
C32 H32 0.9300 .
C33 C34 1.357(11) .
C33 H33 0.9300 .
C34 C35 1.362(11) .
C34 H34 0.9300 .
C35 C36 1.371(9) .
C35 H35 0.9300 .
C36 H36 0.9300 .
