#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/28/4322858.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_4322858
loop_
_publ_author_name
'Paulo Perez-Lourido'
'J. Romero'
'J. Garcia-Vazquez'
'Antonio Sousa'
'Kevin P. Maresca'
'David J. Rose'
'Jon Zubieta'
_publ_section_title
;
 Synthesis and Characterization of Rhenium Phosphinothiolate Complexes.
 Crystal and Molecular Structures of [HNEt3][Re{P(C6H4S)3}2],
 [ReOCl{OP(C6H5)2(C6H4S)}{(P(C6H5)2(C6H4S)}], [Re2O5{P(C6H5)2(C6H4S)}2],
 and [ReOCl{OP(C6H5)2(2-SC6H3-3-SiMe3)}2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3331
_journal_page_last               3336
_journal_paper_doi               10.1021/ic9715299
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C36 H28 Cl O2 P2 Re S2'
_chemical_formula_weight         840.29
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                98.177(1)
_cell_angle_beta                 104.132(1)
_cell_angle_gamma                109.000(1)
_cell_formula_units_Z            2
_cell_length_a                   9.3427(1)
_cell_length_b                   11.9075(1)
_cell_length_c                   16.8504(1)
_cell_measurement_temperature    150(1)
_cell_volume                     1667.80(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11087
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    3.976
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       Plate
_exptl_crystal_F_000             828
_exptl_crystal_size_max          .23
_exptl_crystal_size_mid          .13
_exptl_crystal_size_min          .11
_refine_diff_density_max         1.113
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.099
_refine_ls_goodness_of_fit_obs   1.089
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_restrained_S_obs      1.089
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_obs          0.0333
_refine_ls_shift/esd_max         -2.352
_refine_ls_shift/esd_mean        0.478
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0049P)²+8.1225P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0747
_refine_ls_wR_factor_obs         0.0711
_reflns_number_observed          7014
_reflns_number_total             7567
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9715299_1.cif
_cod_data_source_block           dave152
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0049P)^2^+8.1225P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0049P)^2^+8.1225P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1667.79(2)
_cod_original_formula_sum        'C36 H28 O2 P2 S2 Cl Re'
_cod_database_code               4322858
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re1 Re 0.65262(2) 0.87048(2) 0.751313(11) 0.01492(5) Uani 1 d . .
Cl1 Cl 0.42892(13) 0.72198(10) 0.63188(7) 0.0223(2) Uani 1 d . .
S1 S 0.86764(14) 0.97217(11) 0.87069(7) 0.0245(2) Uani 1 d . .
S2 S 0.52399(13) 0.81614(10) 0.85357(7) 0.0208(2) Uani 1 d . .
P1 P 0.85301(13) 0.89295(10) 0.67890(7) 0.0159(2) Uani 1 d . .
P2 P 0.63367(13) 0.60325(10) 0.79538(7) 0.0152(2) Uani 1 d . .
O1 O 0.6019(4) 0.9836(3) 0.7190(2) 0.0262(7) Uani 1 d . .
O2 O 0.7044(3) 0.7047(3) 0.7543(2) 0.0166(6) Uani 1 d . .
C1 C 0.8420(5) 0.9919(4) 0.6056(3) 0.0189(8) Uani 1 d . .
C2 C 0.6985(6) 0.9623(4) 0.5418(3) 0.0242(9) Uani 1 d . .
H2A H 0.6094(6) 0.8956(4) 0.5388(3) 0.029 Uiso 1 calc R .
C3 C 0.6890(7) 1.0324(5) 0.4830(3) 0.0314(11) Uani 1 d . .
H3A H 0.5946(7) 1.0104(5) 0.4394(3) 0.038 Uiso 1 calc R .
C4 C 0.8189(7) 1.1346(5) 0.4889(3) 0.0326(11) Uani 1 d . .
H4A H 0.8115(7) 1.1821(5) 0.4500(3) 0.039 Uiso 1 calc R .
C5 C 0.9593(7) 1.1657(5) 0.5526(4) 0.0363(12) Uani 1 d . .
H5A H 1.0465(7) 1.2348(5) 0.5567(4) 0.044 Uiso 1 calc R .
C6 C 0.9721(7) 1.0949(4) 0.6110(4) 0.0306(11) Uani 1 d . .
H6A H 1.0677(7) 1.1165(4) 0.6536(4) 0.037 Uiso 1 calc R .
C7 C 0.8528(5) 0.7538(4) 0.6177(3) 0.0166(8) Uani 1 d . .
C8 C 0.9703(5) 0.7082(4) 0.6461(3) 0.0204(9) Uani 1 d . .
H8A H 1.0505(5) 0.7489(4) 0.6970(3) 0.025 Uiso 1 calc R .
C9 C 0.9682(6) 0.6020(4) 0.5985(3) 0.0247(10) Uani 1 d . .
H9A H 1.0481(6) 0.5726(4) 0.6172(3) 0.030 Uiso 1 calc R .
C10 C 0.8473(6) 0.5397(4) 0.5232(3) 0.0235(9) Uani 1 d . .
H10A H 0.8464(6) 0.4688(4) 0.4914(3) 0.028 Uiso 1 calc R .
C11 C 0.7271(6) 0.5833(4) 0.4953(3) 0.0232(9) Uani 1 d . .
H11A H 0.6456(6) 0.5412(4) 0.4450(3) 0.028 Uiso 1 calc R .
C12 C 0.7291(5) 0.6894(4) 0.5425(3) 0.0211(9) Uani 1 d . .
H12A H 0.6483(5) 0.7180(4) 0.5242(3) 0.025 Uiso 1 calc R .
C13 C 1.0456(5) 0.9667(4) 0.7598(3) 0.0205(9) Uani 1 d . .
C14 C 1.1908(5) 0.9893(4) 0.7426(3) 0.0253(10) Uani 1 d . .
H14A H 1.1912(5) 0.9661(4) 0.6876(3) 0.030 Uiso 1 calc R .
C15 C 1.3336(6) 1.0460(5) 0.8075(3) 0.0345(12) Uani 1 d . .
H15A H 1.4298(6) 1.0611(5) 0.7961(3) 0.041 Uiso 1 calc R .
C16 C 1.3319(6) 1.0803(6) 0.8903(4) 0.0392(13) Uani 1 d . .
H16A H 1.4273(6) 1.1176(6) 0.9341(4) 0.047 Uiso 1 calc R .
C17 C 1.1895(6) 1.0592(5) 0.9070(3) 0.0348(12) Uani 1 d . .
H17A H 1.1896(6) 1.0837(5) 0.9620(3) 0.042 Uiso 1 calc R .
C18 C 1.0451(5) 1.0014(4) 0.8424(3) 0.0222(9) Uani 1 d . .
C19 C 0.6530(5) 0.4661(4) 0.7483(3) 0.0188(8) Uani 1 d . .
C20 C 0.6492(5) 0.4454(4) 0.6644(3) 0.0205(9) Uani 1 d . .
H20A H 0.6377(5) 0.5025(4) 0.6335(3) 0.025 Uiso 1 calc R .
C21 C 0.6627(6) 0.3387(4) 0.6264(3) 0.0268(10) Uani 1 d . .
H21A H 0.6602(6) 0.3249(4) 0.5702(3) 0.032 Uiso 1 calc R .
C22 C 0.6798(6) 0.2532(4) 0.6720(4) 0.0302(11) Uani 1 d . .
H22A H 0.6880(6) 0.1821(4) 0.6463(4) 0.036 Uiso 1 calc R .
C23 C 0.6849(6) 0.2735(4) 0.7559(3) 0.0290(11) Uani 1 d . .
H23A H 0.6977(6) 0.2165(4) 0.7866(3) 0.035 Uiso 1 calc R .
C24 C 0.6705(6) 0.3800(4) 0.7945(3) 0.0244(10) Uani 1 d . .
H24A H 0.6727(6) 0.3934(4) 0.8505(3) 0.029 Uiso 1 calc R .
C25 C 0.7442(5) 0.6389(4) 0.9053(3) 0.0202(9) Uani 1 d . .
C26 C 0.9092(5) 0.6971(5) 0.9283(3) 0.0265(10) Uani 1 d . .
H26A H 0.9576(5) 0.7230(5) 0.8885(3) 0.032 Uiso 1 calc R .
C27 C 1.0005(7) 0.7162(5) 1.0107(3) 0.0372(12) Uani 1 d . .
H27A H 1.1107(7) 0.7544(5) 1.0261(3) 0.045 Uiso 1 calc R .
C28 C 0.9295(7) 0.6792(6) 1.0700(4) 0.0444(15) Uani 1 d . .
H28A H 0.9918(7) 0.6922(6) 1.1252(4) 0.053 Uiso 1 calc R .
C29 C 0.7669(7) 0.6231(7) 1.0480(4) 0.048(2) Uani 1 d . .
H29A H 0.7192(7) 0.5989(7) 1.0884(4) 0.058 Uiso 1 calc R .
C30 C 0.6734(6) 0.6024(6) 0.9652(3) 0.0368(13) Uani 1 d . .
H30A H 0.5633(6) 0.5641(6) 0.9503(3) 0.044 Uiso 1 calc R .
C31 C 0.4270(5) 0.5683(4) 0.7852(3) 0.0174(8) Uani 1 d . .
C32 C 0.3122(5) 0.4492(4) 0.7510(3) 0.0229(9) Uani 1 d . .
H32A H 0.3412(5) 0.3859(4) 0.7305(3) 0.028 Uiso 1 calc R .
C33 C 0.1551(5) 0.4263(5) 0.7479(3) 0.0272(10) Uani 1 d . .
H33A H 0.0789(5) 0.3475(5) 0.7247(3) 0.033 Uiso 1 calc R .
C34 C 0.1109(6) 0.5195(5) 0.7789(3) 0.0282(10) Uani 1 d . .
H34A H 0.0059(6) 0.5024(5) 0.7780(3) 0.034 Uiso 1 calc R .
C35 C 0.2230(5) 0.6390(5) 0.8115(3) 0.0249(10) Uani 1 d . .
H35A H 0.1927(5) 0.7014(5) 0.8321(3) 0.030 Uiso 1 calc R .
C36 C 0.3813(5) 0.6647(4) 0.8130(3) 0.0197(9) Uani 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'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O1 Re1 O2 163.46(14) . . ?
O1 Re1 S1 103.48(13) . . ?
O2 Re1 S1 89.12(9) . . ?
O1 Re1 S2 106.75(11) . . ?
O2 Re1 S2 85.44(8) . . ?
S1 Re1 S2 81.61(4) . . ?
O1 Re1 P1 93.91(11) . . ?
O2 Re1 P1 76.40(8) . . ?
S1 Re1 P1 84.58(4) . . ?
S2 Re1 P1 157.31(4) . . ?
O1 Re1 Cl1 88.80(12) . . ?
O2 Re1 Cl1 79.03(8) . . ?
S1 Re1 Cl1 167.68(4) . . ?
S2 Re1 Cl1 93.98(4) . . ?
P1 Re1 Cl1 95.76(4) . . ?
C18 S1 Re1 108.7(2) . . ?
C36 S2 Re1 108.61(14) . . ?
C13 P1 C7 107.4(2) . . ?
C13 P1 C1 107.4(2) . . ?
C7 P1 C1 105.3(2) . . ?
C13 P1 Re1 106.53(15) . . ?
C7 P1 Re1 117.37(14) . . ?
C1 P1 Re1 112.47(14) . . ?
O2 P2 C31 114.2(2) . . ?
O2 P2 C19 109.0(2) . . ?
C31 P2 C19 107.8(2) . . ?
O2 P2 C25 111.1(2) . . ?
C31 P2 C25 108.9(2) . . ?
C19 P2 C25 105.4(2) . . ?
P2 O2 Re1 126.9(2) . . ?
C6 C1 C2 119.0(4) . . ?
C6 C1 P1 122.1(4) . . ?
C2 C1 P1 119.0(3) . . ?
C3 C2 C1 120.1(5) . . ?
C4 C3 C2 120.4(5) . . ?
C3 C4 C5 119.7(5) . . ?
C4 C5 C6 120.7(5) . . ?
C1 C6 C5 120.0(5) . . ?
C8 C7 C12 119.5(4) . . ?
C8 C7 P1 121.1(3) . . ?
C12 C7 P1 119.4(3) . . ?
C7 C8 C9 120.2(4) . . ?
C10 C9 C8 120.2(4) . . ?
C9 C10 C11 120.0(4) . . ?
C12 C11 C10 120.0(4) . . ?
C11 C12 C7 120.1(4) . . ?
C18 C13 C14 119.9(4) . . ?
C18 C13 P1 116.9(3) . . ?
C14 C13 P1 123.2(4) . . ?
C15 C14 C13 120.1(5) . . ?
C14 C15 C16 119.5(5) . . ?
C17 C16 C15 120.3(5) . . ?
C16 C17 C18 120.7(5) . . ?
C13 C18 C17 119.4(4) . . ?
C13 C18 S1 123.1(4) . . ?
C17 C18 S1 117.4(4) . . ?
C20 C19 C24 119.8(4) . . ?
C20 C19 P2 119.1(3) . . ?
C24 C19 P2 121.1(4) . . ?
C19 C20 C21 119.9(4) . . ?
C22 C21 C20 120.3(5) . . ?
C21 C22 C23 120.2(5) . . ?
C22 C23 C24 120.0(4) . . ?
C23 C24 C19 119.8(5) . . ?
C30 C25 C26 119.7(4) . . ?
C30 C25 P2 122.6(4) . . ?
C26 C25 P2 117.5(3) . . ?
C27 C26 C25 119.6(5) . . ?
C28 C27 C26 120.4(5) . . ?
C29 C28 C27 120.3(5) . . ?
C28 C29 C30 120.0(5) . . ?
C25 C30 C29 120.0(5) . . ?
C36 C31 C32 119.9(4) . . ?
C36 C31 P2 118.0(3) . . ?
C32 C31 P2 122.1(3) . . ?
C33 C32 C31 119.7(5) . . ?
C34 C33 C32 120.7(5) . . ?
C33 C34 C35 120.3(4) . . ?
C34 C35 C36 119.8(5) . . ?
C35 C36 C31 119.4(4) . . ?
C35 C36 S2 120.2(4) . . ?
C31 C36 S2 120.4(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
Re1 O1 1.683(3) . ?
Re1 O2 2.184(3) . ?
Re1 S1 2.3018(12) . ?
Re1 S2 2.3777(11) . ?
Re1 P1 2.4388(11) . ?
Re1 Cl1 2.4642(11) . ?
S1 C18 1.777(5) . ?
S2 C36 1.771(5) . ?
P1 C13 1.817(5) . ?
P1 C7 1.822(4) . ?
P1 C1 1.832(4) . ?
P2 O2 1.522(3) . ?
P2 C31 1.796(4) . ?
P2 C19 1.795(5) . ?
P2 C25 1.798(4) . ?
C1 C6 1.391(6) . ?
C1 C2 1.399(6) . ?
C2 C3 1.387(6) . ?
C3 C4 1.382(8) . ?
C4 C5 1.375(8) . ?
C5 C6 1.391(7) . ?
C7 C8 1.390(6) . ?
C7 C12 1.401(6) . ?
C8 C9 1.389(6) . ?
C9 C10 1.386(7) . ?
C10 C11 1.394(7) . ?
C11 C12 1.386(6) . ?
C13 C18 1.395(6) . ?
C13 C14 1.405(6) . ?
C14 C15 1.386(7) . ?
C15 C16 1.403(8) . ?
C16 C17 1.378(8) . ?
C17 C18 1.395(7) . ?
C19 C20 1.390(6) . ?
C19 C24 1.399(6) . ?
C20 C21 1.398(6) . ?
C21 C22 1.385(7) . ?
C22 C23 1.387(8) . ?
C23 C24 1.402(7) . ?
C25 C30 1.382(7) . ?
C25 C26 1.394(6) . ?
C26 C27 1.382(7) . ?
C27 C28 1.377(8) . ?
C28 C29 1.373(8) . ?
C29 C30 1.392(7) . ?
C31 C36 1.408(6) . ?
C31 C32 1.403(6) . ?
C32 C33 1.388(6) . ?
C33 C34 1.384(7) . ?
C34 C35 1.396(7) . ?
C35 C36 1.402(6) . ?
