#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:12:15 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178889 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/18/4111805.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_4111805
loop_
_publ_author_name
'Ming Li'
'Arkady Ellern'
'James H. Espenson'
_publ_section_title
;
 Studies of C-S Bond Cleavage Reactions of Re(V) Dithiolates: Synthesis,
 Reactivity, and Mechanism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10436
_journal_page_last               10447
_journal_paper_doi               10.1021/ja0519334
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C34 H30 Cl O P Re S2'
_chemical_formula_weight         771.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 100.432(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.247(2)
_cell_length_b                   30.973(6)
_cell_length_c                   10.280(2)
_cell_measurement_reflns_used    920
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      24.74
_cell_measurement_theta_min      2.41
_cell_volume                     3208.7(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0668
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26813
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    4.076
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.072
_refine_diff_density_min         -2.754
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0502
_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)+(0.0457P)²+8.7418P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                4975
_reflns_number_total             6566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0519334si20050408_011907.cif
_cod_data_source_block           esp73
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3208.8(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4111805
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.19883(3) 0.115825(8) 0.67870(3) 0.03029(10) Uani 1 1 d .
P1 P 0.26960(18) 0.11453(5) 0.45975(18) 0.0304(4) Uani 1 1 d .
S1 S 0.15644(19) 0.13949(7) 0.8807(2) 0.0425(5) Uani 1 1 d .
S2 S 0.01777(19) 0.14892(7) 0.56908(19) 0.0406(4) Uani 1 1 d .
C1 C 0.4412(7) 0.1004(2) 0.4705(8) 0.0348(16) Uani 1 1 d .
C2 C 0.4885(9) 0.0637(3) 0.5438(9) 0.051(2) Uani 1 1 d .
H2 H 0.4314 0.0482 0.5888 0.061 Uiso 1 1 calc R
C3 C 0.6171(9) 0.0499(3) 0.5510(11) 0.065(3) Uani 1 1 d .
H3 H 0.6469 0.0249 0.5994 0.078 Uiso 1 1 calc R
C4 C 0.7015(9) 0.0725(3) 0.4878(12) 0.071(3) Uani 1 1 d .
H4 H 0.7892 0.0629 0.4920 0.085 Uiso 1 1 calc R
C5 C 0.6594(9) 0.1086(3) 0.4190(11) 0.070(3) Uani 1 1 d .
H5 H 0.7190 0.1244 0.3777 0.084 Uiso 1 1 calc R
C6 C 0.5314(8) 0.1227(3) 0.4087(9) 0.052(2) Uani 1 1 d .
H6 H 0.5038 0.1476 0.3593 0.062 Uiso 1 1 calc R
C7 C 0.2451(7) 0.1648(2) 0.3679(7) 0.0332(16) Uani 1 1 d .
C8 C 0.2938(9) 0.2031(2) 0.4306(8) 0.046(2) Uani 1 1 d .
H8 H 0.3411 0.2026 0.5179 0.055 Uiso 1 1 calc R
C9 C 0.2716(9) 0.2418(2) 0.3624(9) 0.050(2) Uani 1 1 d .
H9 H 0.3037 0.2677 0.4042 0.061 Uiso 1 1 calc R
C10 C 0.2052(9) 0.2428(2) 0.2380(9) 0.048(2) Uani 1 1 d .
H10 H 0.1925 0.2694 0.1935 0.057 Uiso 1 1 calc R
C11 C 0.1548(10) 0.2057(3) 0.1732(9) 0.054(2) Uani 1 1 d .
H11 H 0.1072 0.2068 0.0860 0.065 Uiso 1 1 calc R
C12 C 0.1763(8) 0.1666(2) 0.2403(8) 0.0430(19) Uani 1 1 d .
H12 H 0.1433 0.1410 0.1975 0.052 Uiso 1 1 calc R
C13 C 0.1830(7) 0.0723(2) 0.3542(7) 0.0324(15) Uani 1 1 d .
C14 C 0.2414(8) 0.0533(2) 0.2580(8) 0.0429(19) Uani 1 1 d .
H14 H 0.3239 0.0633 0.2424 0.052 Uiso 1 1 calc R
C15 C 0.1778(10) 0.0194(3) 0.1845(10) 0.061(3) Uani 1 1 d .
H15 H 0.2181 0.0067 0.1187 0.073 Uiso 1 1 calc R
C16 C 0.0604(11) 0.0043(3) 0.2044(10) 0.065(3) Uani 1 1 d .
H16 H 0.0194 -0.0189 0.1537 0.078 Uiso 1 1 calc R
C17 C 0.0008(11) 0.0229(3) 0.2991(11) 0.075(3) Uani 1 1 d .
H17 H -0.0817 0.0128 0.3141 0.090 Uiso 1 1 calc R
C18 C 0.0643(9) 0.0571(3) 0.3734(9) 0.058(3) Uani 1 1 d .
H18 H 0.0233 0.0700 0.4385 0.070 Uiso 1 1 calc R
C19 C -0.0831(9) 0.1736(2) 0.6812(9) 0.049(2) Uani 1 1 d .
H19A H -0.0353 0.1986 0.7247 0.059 Uiso 1 1 calc R
H19B H -0.1665 0.1841 0.6286 0.059 Uiso 1 1 calc R
C20 C -0.1141(8) 0.1437(2) 0.7842(8) 0.0413(18) Uani 1 1 d .
C21 C -0.2443(7) 0.1320(3) 0.7890(9) 0.048(2) Uani 1 1 d .
H21 H -0.3140 0.1433 0.7261 0.057 Uiso 1 1 calc R
C22 C -0.2726(9) 0.1041(3) 0.8845(10) 0.057(2) Uani 1 1 d .
H22 H -0.3607 0.0956 0.8845 0.069 Uiso 1 1 calc R
C23 C -0.1719(9) 0.0885(3) 0.9797(9) 0.052(2) Uani 1 1 d .
H23 H -0.1915 0.0701 1.0462 0.063 Uiso 1 1 calc R
C24 C -0.0430(9) 0.0998(3) 0.9778(8) 0.0448(19) Uani 1 1 d .
H24 H 0.0252 0.0889 1.0431 0.054 Uiso 1 1 calc R
C25 C -0.0114(8) 0.1272(2) 0.8810(7) 0.0373(17) Uani 1 1 d .
C26 C 0.8285(13) 0.2133(4) 0.2811(15) 0.086(4) Uani 1 1 d .
H26 H 0.9196 0.2112 0.3161 0.103 Uiso 1 1 calc R
C27 C 0.7756(17) 0.1900(5) 0.1743(16) 0.101(5) Uani 1 1 d .
H27 H 0.8304 0.1723 0.1331 0.121 Uiso 1 1 calc R
C28 C 0.6446(19) 0.1919(6) 0.1259(15) 0.119(5) Uani 1 1 d .
H28 H 0.6071 0.1738 0.0557 0.142 Uiso 1 1 calc R
C29 C 0.5652(16) 0.2205(6) 0.1793(18) 0.119(6) Uani 1 1 d .
H29 H 0.4748 0.2236 0.1426 0.143 Uiso 1 1 calc R
C30 C 0.6212(19) 0.2436(5) 0.285(2) 0.115(5) Uani 1 1 d .
H30 H 0.5679 0.2630 0.3231 0.138 Uiso 1 1 calc R
C31 C 0.7487(19) 0.2402(5) 0.3390(16) 0.110(5) Uani 1 1 d .
H31 H 0.7840 0.2560 0.4154 0.132 Uiso 1 1 calc R
C32 C 0.5233(15) 0.0366(5) 1.0741(17) 0.100(4) Uani 1 1 d .
H32 H 0.5376 0.0618 1.1258 0.120 Uiso 1 1 calc R
C33 C 0.4342(15) 0.0360(5) 0.9596(19) 0.113(5) Uani 1 1 d .
H33 H 0.3892 0.0616 0.9302 0.135 Uiso 1 1 calc R
C34 C 0.4083(14) 0.0005(6) 0.8874(14) 0.101(5) Uani 1 1 d .
H34 H 0.3432 0.0008 0.8101 0.121 Uiso 1 1 calc R
Cl10 Cl 0.39994(18) 0.15032(6) 0.7541(2) 0.0449(5) Uani 1 1 d .
O1 O 0.1865(5) 0.06197(15) 0.6841(5) 0.0449(13) 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'
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'
O O 0.0106 0.0060 '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
O1 Re1 S2 114.3(2) . .
O1 Re1 S1 104.95(19) . .
S2 Re1 S1 91.93(7) . .
O1 Re1 Cl10 120.9(2) . .
S2 Re1 Cl10 124.15(7) . .
S1 Re1 Cl10 81.63(7) . .
O1 Re1 P1 92.87(19) . .
S2 Re1 P1 84.41(7) . .
S1 Re1 P1 161.68(7) . .
Cl10 Re1 P1 85.59(7) . .
C1 P1 C7 106.4(3) . .
C1 P1 C13 103.2(3) . .
C7 P1 C13 107.4(3) . .
C1 P1 Re1 113.0(3) . .
C7 P1 Re1 114.9(2) . .
C13 P1 Re1 111.1(2) . .
C25 S1 Re1 105.9(2) . .
C19 S2 Re1 112.4(3) . .
C6 C1 C2 116.9(7) . .
C6 C1 P1 125.0(6) . .
C2 C1 P1 118.1(6) . .
C3 C2 C1 121.1(8) . .
C3 C2 H2 119.5 . .
C1 C2 H2 119.5 . .
C4 C3 C2 120.0(9) . .
C4 C3 H3 120.0 . .
C2 C3 H3 120.0 . .
C5 C4 C3 120.2(8) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C4 C5 C6 120.9(9) . .
C4 C5 H5 119.5 . .
C6 C5 H5 119.5 . .
C5 C6 C1 120.9(8) . .
C5 C6 H6 119.6 . .
C1 C6 H6 119.6 . .
C12 C7 C8 118.9(7) . .
C12 C7 P1 122.1(5) . .
C8 C7 P1 119.0(6) . .
C9 C8 C7 119.2(8) . .
C9 C8 H8 120.4 . .
C7 C8 H8 120.4 . .
C10 C9 C8 120.8(8) . .
C10 C9 H9 119.6 . .
C8 C9 H9 119.6 . .
C9 C10 C11 121.6(7) . .
C9 C10 H10 119.2 . .
C11 C10 H10 119.2 . .
C10 C11 C12 118.2(8) . .
C10 C11 H11 120.9 . .
C12 C11 H11 120.9 . .
C7 C12 C11 121.2(7) . .
C7 C12 H12 119.4 . .
C11 C12 H12 119.4 . .
C18 C13 C14 118.4(7) . .
C18 C13 P1 121.1(6) . .
C14 C13 P1 120.4(6) . .
C13 C14 C15 119.5(8) . .
C13 C14 H14 120.2 . .
C15 C14 H14 120.2 . .
C16 C15 C14 121.9(8) . .
C16 C15 H15 119.1 . .
C14 C15 H15 119.1 . .
C15 C16 C17 119.3(8) . .
C15 C16 H16 120.3 . .
C17 C16 H16 120.3 . .
C16 C17 C18 119.1(9) . .
C16 C17 H17 120.5 . .
C18 C17 H17 120.5 . .
C13 C18 C17 121.8(8) . .
C13 C18 H18 119.1 . .
C17 C18 H18 119.1 . .
C20 C19 S2 113.8(5) . .
C20 C19 H19A 108.8 . .
S2 C19 H19A 108.8 . .
C20 C19 H19B 108.8 . .
S2 C19 H19B 108.8 . .
H19A C19 H19B 107.7 . .
C21 C20 C25 118.6(8) . .
C21 C20 C19 121.2(8) . .
C25 C20 C19 120.2(7) . .
C22 C21 C20 121.0(8) . .
C22 C21 H21 119.5 . .
C20 C21 H21 119.5 . .
C23 C22 C21 119.9(8) . .
C23 C22 H22 120.0 . .
C21 C22 H22 120.0 . .
C24 C23 C22 120.2(8) . .
C24 C23 H23 119.9 . .
C22 C23 H23 119.9 . .
C23 C24 C25 121.0(8) . .
C23 C24 H24 119.5 . .
C25 C24 H24 119.5 . .
C24 C25 C20 119.2(7) . .
C24 C25 S1 119.1(6) . .
C20 C25 S1 121.7(6) . .
C27 C26 C31 119.7(14) . .
C27 C26 H26 120.2 . .
C31 C26 H26 120.2 . .
C26 C27 C28 120.5(13) . .
C26 C27 H27 119.8 . .
C28 C27 H27 119.8 . .
C27 C28 C29 120.1(17) . .
C27 C28 H28 120.0 . .
C29 C28 H28 120.0 . .
C30 C29 C28 117.9(16) . .
C30 C29 H29 121.0 . .
C28 C29 H29 121.0 . .
C31 C30 C29 122.6(16) . .
C31 C30 H30 118.7 . .
C29 C30 H30 118.7 . .
C30 C31 C26 119.1(16) . .
C30 C31 H31 120.5 . .
C26 C31 H31 120.5 . .
C33 C32 C34 118.1(15) . 3_657
C33 C32 H32 121.0 . .
C34 C32 H32 121.0 3_657 .
C34 C33 C32 122.2(14) . .
C34 C33 H33 118.9 . .
C32 C33 H33 118.9 . .
C33 C34 C32 119.7(14) . 3_657
C33 C34 H34 120.2 . .
C32 C34 H34 120.2 3_657 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 O1 1.675(5) .
Re1 S2 2.2373(19) .
Re1 S1 2.317(2) .
Re1 Cl10 2.3262(18) .
Re1 P1 2.4868(18) .
P1 C1 1.796(7) .
P1 C7 1.814(7) .
P1 C13 1.823(7) .
S1 C25 1.763(8) .
S2 C19 1.848(8) .
C1 C6 1.395(10) .
C1 C2 1.402(11) .
C2 C3 1.374(12) .
C2 H2 0.9400 .
C3 C4 1.365(14) .
C3 H3 0.9400 .
C4 C5 1.353(14) .
C4 H4 0.9400 .
C5 C6 1.368(12) .
C5 H5 0.9400 .
C6 H6 0.9400 .
C7 C12 1.373(10) .
C7 C8 1.399(10) .
C8 C9 1.387(11) .
C8 H8 0.9400 .
C9 C10 1.335(11) .
C9 H9 0.9400 .
C10 C11 1.381(12) .
C10 H10 0.9400 .
C11 C12 1.391(10) .
C11 H11 0.9400 .
C12 H12 0.9400 .
C13 C18 1.352(11) .
C13 C14 1.377(10) .
C14 C15 1.386(11) .
C14 H14 0.9400 .
C15 C16 1.341(13) .
C15 H15 0.9400 .
C16 C17 1.366(14) .
C16 H16 0.9400 .
C17 C18 1.397(11) .
C17 H17 0.9400 .
C18 H18 0.9400 .
C19 C20 1.484(11) .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C20 C21 1.392(10) .
C20 C25 1.407(11) .
C21 C22 1.378(12) .
C21 H21 0.9400 .
C22 C23 1.374(13) .
C22 H22 0.9400 .
C23 C24 1.369(11) .
C23 H23 0.9400 .
C24 C25 1.389(11) .
C24 H24 0.9400 .
C26 C27 1.343(18) .
C26 C31 1.376(19) .
C26 H26 0.9400 .
C27 C28 1.35(2) .
C27 H27 0.9400 .
C28 C29 1.38(2) .
C28 H28 0.9400 .
C29 C30 1.34(2) .
C29 H29 0.9400 .
C30 C31 1.33(2) .
C30 H30 0.9400 .
C31 H31 0.9400 .
C32 C33 1.353(19) .
C32 C34 1.367(19) 3_657
C32 H32 0.9400 .
C33 C34 1.33(2) .
C33 H33 0.9400 .
C34 C32 1.367(19) 3_657
C34 H34 0.9400 .
