#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/71/4327120.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_4327120
loop_
_publ_author_name
'Stephen Sproules'
'Thomas Weyhermüller'
'Richard Goddard'
'Karl Wieghardt'
_publ_section_title
;
 The Rhenium Tris(dithiolene) Electron Transfer Series: Calibrating
 Covalency
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12623
_journal_page_last               12631
_journal_paper_doi               10.1021/ic2016534
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        dichloromethane/pentane
_chemical_formula_moiety         '2(C24 H20 P), C12 N6 Re S6'
_chemical_formula_sum            'C60 H40 N6 P2 Re S6'
_chemical_formula_weight         1285.48
_chemical_name_systematic
; 
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                WGT-SS-086-01
_audit_creation_date             2008-07-02
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.032(8)
_cell_length_b                   15.316(6)
_cell_length_c                   18.062(7)
_cell_measurement_reflns_used    9718
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      37.53
_cell_measurement_theta_min      2.77
_cell_volume                     5542(4)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2004)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 18.18
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX-II'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'ANKA synchrotron source, Karlsruhe'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            197019
_diffrn_reflns_theta_full        33.13
_diffrn_reflns_theta_max         33.13
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    2.522
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.7034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (G. M. Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             2572
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.652
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         7220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.0482
_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)+(0.0000P)²+10.6536P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                6030
_reflns_number_total             7224
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic2016534_si_002_3.cif
_cod_data_source_block           6281
_cod_original_sg_symbol_Hall     '-p 2n 2ab'
_cod_database_code               4327120
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C12 C 0.61289(15) 0.76912(19) 0.14918(19) 0.0273(6) Uani 1 1 d .
C15 C 0.64948(16) 0.7978(2) 0.08530(19) 0.0306(7) Uani 1 1 d .
C2 C 0.47728(18) 0.4572(2) 0.2223(2) 0.0350(7) Uani 1 1 d .
C5 C 0.4538(2) 0.3782(3) 0.1893(2) 0.0463(9) Uani 1 1 d .
N16 N 0.67844(17) 0.8192(2) 0.03364(19) 0.0425(7) Uani 1 1 d .
N6 N 0.4346(2) 0.3147(2) 0.1622(3) 0.0658(11) Uani 1 1 d .
Re1 Re 0.5000 0.667616(11) 0.2500 0.02746(6) Uani 1 2 d S
S11 S 0.55171(4) 0.69127(5) 0.13391(4) 0.02862(16) Uani 1 1 d .
S1 S 0.44567(4) 0.55427(5) 0.18675(5) 0.03123(17) Uani 1 1 d .
C13 C 0.62649(16) 0.8009(2) 0.21801(19) 0.0282(6) Uani 1 1 d .
C17 C 0.67947(18) 0.8620(2) 0.2286(2) 0.0332(7) Uani 1 1 d .
N18 N 0.72183(19) 0.9115(2) 0.2359(2) 0.0507(9) Uani 1 1 d .
S14 S 0.58273(4) 0.76564(5) 0.29508(5) 0.02825(16) Uani 1 1 d .
P20 P 0.63337(4) 0.16515(5) 0.09565(4) 0.02461(16) Uani 1 1 d .
C21 C 0.55829(15) 0.1013(2) 0.10379(18) 0.0269(6) Uani 1 1 d .
C22 C 0.56157(17) 0.0221(2) 0.1425(2) 0.0338(7) Uani 1 1 d .
H22 H 0.6017 0.0057 0.1668 0.041 Uiso 1 1 calc R
C23 C 0.50659(17) -0.0322(2) 0.1453(2) 0.0385(8) Uani 1 1 d .
H23 H 0.5089 -0.0859 0.1716 0.046 Uiso 1 1 calc R
C24 C 0.44825(17) -0.0082(2) 0.1099(2) 0.0363(8) Uani 1 1 d .
H24 H 0.4105 -0.0457 0.1117 0.044 Uiso 1 1 calc R
C25 C 0.44454(18) 0.0695(2) 0.0722(2) 0.0388(8) Uani 1 1 d .
H25 H 0.4042 0.0854 0.0481 0.047 Uiso 1 1 calc R
C26 C 0.49940(17) 0.1250(2) 0.0689(2) 0.0348(7) Uani 1 1 d .
H26 H 0.4965 0.1788 0.0430 0.042 Uiso 1 1 calc R
C31 C 0.61732(16) 0.2797(2) 0.08306(18) 0.0277(6) Uani 1 1 d .
C32 C 0.58300(19) 0.3097(2) 0.0207(2) 0.0356(8) Uani 1 1 d .
H32 H 0.5676 0.2698 -0.0157 0.043 Uiso 1 1 calc R
C33 C 0.5716(2) 0.3989(2) 0.0126(2) 0.0418(8) Uani 1 1 d .
H33 H 0.5473 0.4198 -0.0290 0.050 Uiso 1 1 calc R
C34 C 0.59546(19) 0.4572(2) 0.0645(2) 0.0406(9) Uani 1 1 d .
H34 H 0.5879 0.5180 0.0583 0.049 Uiso 1 1 calc R
C35 C 0.6301(2) 0.4277(2) 0.1251(2) 0.0386(8) Uani 1 1 d .
H35 H 0.6467 0.4683 0.1604 0.046 Uiso 1 1 calc R
C36 C 0.64129(17) 0.3386(2) 0.13537(19) 0.0320(7) Uani 1 1 d .
H36 H 0.6650 0.3184 0.1776 0.038 Uiso 1 1 calc R
C41 C 0.68127(16) 0.1502(2) 0.17848(17) 0.0266(6) Uani 1 1 d .
C42 C 0.65066(19) 0.1614(2) 0.24748(19) 0.0343(7) Uani 1 1 d .
H42 H 0.6042 0.1730 0.2506 0.041 Uiso 1 1 calc R
C43 C 0.6890(2) 0.1553(2) 0.3112(2) 0.0377(8) Uani 1 1 d .
H43 H 0.6689 0.1634 0.3584 0.045 Uiso 1 1 calc R
C44 C 0.75658(19) 0.1374(2) 0.30607(19) 0.0361(8) Uani 1 1 d .
H44 H 0.7827 0.1339 0.3498 0.043 Uiso 1 1 calc R
C45 C 0.78632(18) 0.1246(2) 0.23826(19) 0.0331(7) Uani 1 1 d .
H45 H 0.8325 0.1110 0.2355 0.040 Uiso 1 1 calc R
C46 C 0.74902(16) 0.13151(19) 0.17405(18) 0.0267(6) Uani 1 1 d .
H46 H 0.7696 0.1235 0.1272 0.032 Uiso 1 1 calc R
C51 C 0.68279(16) 0.1254(2) 0.01997(17) 0.0271(6) Uani 1 1 d .
C52 C 0.69660(17) 0.0360(2) 0.01741(19) 0.0317(7) Uani 1 1 d .
H52 H 0.6759 -0.0024 0.0517 0.038 Uiso 1 1 calc R
C53 C 0.74040(19) 0.0036(2) -0.03497(19) 0.0365(8) Uani 1 1 d .
H53 H 0.7501 -0.0571 -0.0364 0.044 Uiso 1 1 calc R
C54 C 0.7700(2) 0.0595(3) -0.0852(2) 0.0449(9) Uani 1 1 d .
H54 H 0.8002 0.0372 -0.1211 0.054 Uiso 1 1 calc R
C55 C 0.7560(2) 0.1476(3) -0.0833(2) 0.0500(10) Uani 1 1 d .
H55 H 0.7761 0.1856 -0.1184 0.060 Uiso 1 1 calc R
C56 C 0.7128(2) 0.1811(2) -0.0305(2) 0.0395(8) Uani 1 1 d .
H56 H 0.7038 0.2420 -0.0289 0.047 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'
P P 0.1023 0.0942 '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'
S S 0.1246 0.1234 '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 C12 C15 121.5(3) . .
C13 C12 S11 122.2(3) . .
C15 C12 S11 116.3(3) . .
N16 C15 C12 178.7(4) . .
C2 C2 C5 122.0(2) 3_655 .
C2 C2 S1 121.21(13) 3_655 .
C5 C2 S1 116.7(3) . .
N6 C5 C2 179.4(6) . .
S1 Re1 S1 84.53(5) . 3_655
S1 Re1 S11 83.39(3) . .
S1 Re1 S11 109.98(3) 3_655 .
S1 Re1 S11 109.98(3) . 3_655
S1 Re1 S11 83.39(3) 3_655 3_655
S11 Re1 S11 162.39(4) . 3_655
S1 Re1 S14 163.04(3) . .
S1 Re1 S14 88.69(4) 3_655 .
S11 Re1 S14 84.36(3) . .
S11 Re1 S14 84.56(3) 3_655 .
S1 Re1 S14 88.69(4) . 3_655
S1 Re1 S14 163.04(3) 3_655 3_655
S11 Re1 S14 84.56(3) . 3_655
S11 Re1 S14 84.36(3) 3_655 3_655
S14 Re1 S14 101.77(5) . 3_655
C12 S11 Re1 105.90(12) . .
C2 S1 Re1 106.50(13) . .
C12 C13 C17 120.4(3) . .
C12 C13 S14 121.4(2) . .
C17 C13 S14 118.2(3) . .
N18 C17 C13 178.8(4) . .
C13 S14 Re1 105.93(12) . .
C41 P20 C51 107.30(15) . .
C41 P20 C31 109.01(15) . .
C51 P20 C31 109.48(15) . .
C41 P20 C21 108.05(15) . .
C51 P20 C21 109.80(14) . .
C31 P20 C21 113.03(15) . .
C26 C21 C22 119.6(3) . .
C26 C21 P20 122.1(3) . .
C22 C21 P20 118.2(2) . .
C23 C22 C21 120.2(3) . .
C22 C23 C24 119.8(3) . .
C25 C24 C23 120.4(3) . .
C24 C25 C26 120.5(3) . .
C21 C26 C25 119.6(3) . .
C36 C31 C32 120.2(3) . .
C36 C31 P20 119.0(3) . .
C32 C31 P20 120.7(2) . .
C33 C32 C31 119.3(3) . .
C34 C33 C32 120.4(3) . .
C35 C34 C33 120.3(3) . .
C34 C35 C36 120.6(3) . .
C31 C36 C35 119.3(3) . .
C46 C41 C42 120.3(3) . .
C46 C41 P20 120.1(2) . .
C42 C41 P20 119.6(3) . .
C43 C42 C41 119.3(3) . .
C44 C43 C42 119.9(3) . .
C45 C44 C43 120.8(3) . .
C44 C45 C46 120.1(3) . .
C45 C46 C41 119.7(3) . .
C56 C51 C52 119.7(3) . .
C56 C51 P20 122.1(3) . .
C52 C51 P20 117.8(2) . .
C53 C52 C51 120.0(3) . .
C54 C53 C52 120.0(3) . .
C55 C54 C53 120.2(4) . .
C54 C55 C56 120.4(3) . .
C51 C56 C55 119.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C12 C13 1.363(5) .
C12 C15 1.436(5) .
C12 S11 1.732(3) .
C15 N16 1.147(4) .
C2 C2 1.352(8) 3_655
C2 C5 1.428(5) .
C2 S1 1.739(4) .
C5 N6 1.155(5) .
Re1 S1 2.3459(10) .
Re1 S1 2.3459(10) 3_655
Re1 S11 2.3667(11) .
Re1 S11 2.3667(11) 3_655
Re1 S14 2.3797(10) .
Re1 S14 2.3798(10) 3_655
C13 C17 1.428(5) .
C13 S14 1.732(3) .
C17 N18 1.145(5) .
P20 C41 1.792(3) .
P20 C51 1.794(3) .
P20 C31 1.798(3) .
P20 C21 1.800(3) .
C21 C26 1.386(4) .
C21 C22 1.401(4) .
C22 C23 1.381(5) .
C23 C24 1.382(5) .
C24 C25 1.373(5) .
C25 C26 1.391(5) .
C31 C36 1.392(4) .
C31 C32 1.397(5) .
C32 C33 1.393(5) .
C33 C34 1.380(5) .
C34 C35 1.373(5) .
C35 C36 1.395(5) .
C41 C46 1.390(4) .
C41 C42 1.399(5) .
C42 C43 1.387(5) .
C43 C44 1.385(5) .
C44 C45 1.376(5) .
C45 C46 1.384(4) .
C51 C56 1.385(5) .
C51 C52 1.397(4) .
C52 C53 1.383(5) .
C53 C54 1.382(5) .
C54 C55 1.378(5) .
C55 C56 1.387(5) .
