#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:22:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179324 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/21/4322146.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_4322146
loop_
_publ_author_name
'Josemon Jacob'
'Ilia A. Guzei'
'James H. Espenson'
_publ_contact_author_address
;
   Department of Chemistry
   Iowa State University of Science and Technology
   Ames, Iowa, 50011
   USA
;
_publ_contact_author_email       iguzei@iastate.edu
_publ_contact_author_fax         +515-294-5717
_publ_contact_author_name
;
Ilia A. Guzei
;
_publ_contact_author_phone       +515-294-6419
_publ_section_title
;
 Synthesis and Structural Characterization of Novel Terminal and Bridging
 Re(V)-Sulfido Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3266
_journal_page_last               3267
_journal_paper_doi               10.1021/ic990354v
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C16 H18 O Re2 S5'
_chemical_formula_weight         759.00
_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                 90.4230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2214(6)
_cell_length_b                   12.8234(7)
_cell_length_c                   13.7784(8)
_cell_measurement_temperature    193(2)
_cell_volume                     1982.61(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3839
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    12.728
_exptl_absorpt_correction_T_max  0.3938
_exptl_absorpt_correction_T_min  0.0778
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0252P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.0466
_reflns_number_gt                3334
_reflns_number_total             3839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990354v_2.cif
_cod_data_source_block           esp11tm
_cod_database_code               4322146
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.803046(18) 0.846177(13) 0.504785(11) 0.02236(6) Uani 1 1 d . . .
Re2 Re 0.952113(17) 0.714463(12) 0.609915(11) 0.01961(6) Uani 1 1 d . . .
S1 S 0.77629(11) 0.78751(8) 0.66727(7) 0.0220(2) Uani 1 1 d . . .
S2 S 0.72776(13) 1.00683(8) 0.55384(8) 0.0298(3) Uani 1 1 d . . .
S3 S 1.04338(12) 0.79221(8) 0.73660(7) 0.0256(3) Uani 1 1 d . . .
S4 S 1.10334(12) 0.59270(8) 0.59895(8) 0.0269(3) Uani 1 1 d . . .
S5 S 0.99105(12) 0.78511(9) 0.46895(7) 0.0279(3) Uani 1 1 d . . .
O O 0.7029(3) 0.7775(2) 0.4406(2) 0.0342(8) Uani 1 1 d . . .
C1 C 0.8651(5) 0.9589(4) 0.3975(3) 0.0339(12) Uani 1 1 d . . .
H1A H 0.8946 0.9217 0.3403 0.051 Uiso 1 1 calc R . .
H1B H 0.9296 1.0009 0.4257 0.051 Uiso 1 1 calc R . .
H1C H 0.7990 1.0046 0.3783 0.051 Uiso 1 1 calc R . .
C2 C 0.8457(5) 0.5762(3) 0.6127(3) 0.0304(11) Uani 1 1 d . . .
H2A H 0.8043 0.5682 0.5503 0.046 Uiso 1 1 calc R . .
H2B H 0.7870 0.5816 0.6648 0.046 Uiso 1 1 calc R . .
H2C H 0.8970 0.5156 0.6243 0.046 Uiso 1 1 calc R . .
C3 C 0.7893(5) 0.8997(3) 0.7507(3) 0.0265(11) Uani 1 1 d . . .
H3A H 0.8057 0.8753 0.8177 0.032 Uiso 1 1 calc R . .
H3B H 0.8552 0.9460 0.7305 0.032 Uiso 1 1 calc R . .
C4 C 0.6742(4) 0.9568(3) 0.7468(3) 0.0241(10) Uani 1 1 d . . .
C5 C 0.6003(5) 0.9633(3) 0.8274(3) 0.0285(11) Uani 1 1 d . . .
H5 H 0.6230 0.9299 0.8862 0.034 Uiso 1 1 calc R . .
C6 C 0.4944(5) 1.0180(3) 0.8223(3) 0.0323(11) Uani 1 1 d . . .
H6 H 0.4454 1.0229 0.8781 0.039 Uiso 1 1 calc R . .
C7 C 0.4590(5) 1.0657(4) 0.7367(4) 0.0379(13) Uani 1 1 d . . .
H7 H 0.3865 1.1039 0.7338 0.045 Uiso 1 1 calc R . .
C8 C 0.5303(5) 1.0574(3) 0.6554(3) 0.0336(12) Uani 1 1 d . . .
H8 H 0.5055 1.0885 0.5960 0.040 Uiso 1 1 calc R . .
C9 C 0.6380(5) 1.0037(3) 0.6604(3) 0.0264(11) Uani 1 1 d . . .
C10 C 1.1924(5) 0.7371(4) 0.7572(3) 0.0322(12) Uani 1 1 d . . .
H10A H 1.2335 0.7793 0.8075 0.039 Uiso 1 1 calc R . .
H10B H 1.1834 0.6656 0.7833 0.039 Uiso 1 1 calc R . .
C11 C 1.2698(5) 0.7323(3) 0.6697(3) 0.0264(11) Uani 1 1 d . . .
C12 C 1.3721(5) 0.7902(4) 0.6615(3) 0.0343(12) Uani 1 1 d . . .
H12 H 1.3944 0.8363 0.7126 0.041 Uiso 1 1 calc R . .
C13 C 1.4438(5) 0.7827(4) 0.5797(4) 0.0375(12) Uani 1 1 d . . .
H13 H 1.5143 0.8232 0.5750 0.045 Uiso 1 1 calc R . .
C14 C 1.4115(5) 0.7157(3) 0.5055(3) 0.0326(12) Uani 1 1 d . . .
H14 H 1.4605 0.7096 0.4498 0.039 Uiso 1 1 calc R . .
C15 C 1.3094(5) 0.6584(3) 0.5119(3) 0.0286(11) Uani 1 1 d . . .
H15 H 1.2878 0.6126 0.4605 0.034 Uiso 1 1 calc R . .
C16 C 1.2364(4) 0.6664(3) 0.5932(3) 0.0236(10) 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'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
O Re1 C1 101.95(17) . . ?
O Re1 S5 108.65(12) . . ?
C1 Re1 S5 77.47(14) . . ?
O Re1 S2 112.02(13) . . ?
C1 Re1 S2 74.31(13) . . ?
S5 Re1 S2 134.16(5) . . ?
O Re1 S1 103.93(11) . . ?
C1 Re1 S1 152.56(13) . . ?
S5 Re1 S1 102.46(4) . . ?
S2 Re1 S1 87.60(4) . . ?
O Re1 Re2 110.76(12) . . ?
C1 Re1 Re2 124.14(14) . . ?
S5 Re1 Re2 49.99(3) . . ?
S2 Re1 Re2 127.23(3) . . ?
S1 Re1 Re2 52.96(3) . . ?
C2 Re2 S5 118.30(13) . . ?
C2 Re2 S3 127.20(13) . . ?
S5 Re2 S3 114.33(4) . . ?
C2 Re2 S4 81.47(14) . . ?
S5 Re2 S4 94.02(4) . . ?
S3 Re2 S4 91.14(4) . . ?
C2 Re2 S1 81.52(13) . . ?
S5 Re2 S1 108.05(4) . . ?
S3 Re2 S1 86.58(4) . . ?
S4 Re2 S1 156.71(4) . . ?
C2 Re2 Re1 100.32(14) . . ?
S5 Re2 Re1 53.79(3) . . ?
S3 Re2 Re1 113.83(3) . . ?
S4 Re2 Re1 144.71(3) . . ?
S1 Re2 Re1 54.80(2) . . ?
C3 S1 Re2 117.49(18) . . ?
C3 S1 Re1 109.22(14) . . ?
Re2 S1 Re1 72.25(3) . . ?
C9 S2 Re1 115.25(14) . . ?
C10 S3 Re2 111.00(14) . . ?
C16 S4 Re2 105.20(14) . . ?
Re2 S5 Re1 76.22(4) . . ?
C4 C3 S1 107.2(3) . . ?
C9 C4 C5 119.0(5) . . ?
C9 C4 C3 119.5(4) . . ?
C5 C4 C3 121.5(4) . . ?
C6 C5 C4 120.4(4) . . ?
C5 C6 C7 120.6(5) . . ?
C6 C7 C8 119.4(5) . . ?
C7 C8 C9 120.3(5) . . ?
C4 C9 C8 120.2(4) . . ?
C4 C9 S2 123.4(4) . . ?
C8 C9 S2 116.3(3) . . ?
C11 C10 S3 115.2(3) . . ?
C12 C11 C16 119.0(4) . . ?
C12 C11 C10 122.4(4) . . ?
C16 C11 C10 118.6(4) . . ?
C11 C12 C13 121.1(5) . . ?
C14 C13 C12 119.5(5) . . ?
C15 C14 C13 120.2(5) . . ?
C14 C15 C16 120.7(4) . . ?
C15 C16 C11 119.5(4) . . ?
C15 C16 S4 119.8(3) . . ?
C11 C16 S4 120.7(4) . . ?
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 O 1.675(3) . ?
Re1 C1 2.185(4) . ?
Re1 S5 2.3072(13) . ?
Re1 S2 2.3288(11) . ?
Re1 S1 2.3828(10) . ?
Re1 Re2 2.7773(3) . ?
Re2 C2 2.138(4) . ?
Re2 S5 2.1901(10) . ?
Re2 S3 2.2502(11) . ?
Re2 S4 2.3118(12) . ?
Re2 S1 2.3276(12) . ?
S1 C3 1.847(4) . ?
S2 C9 1.787(5) . ?
S3 C10 1.836(5) . ?
S4 C16 1.769(5) . ?
C3 C4 1.485(7) . ?
C4 C9 1.392(6) . ?
C4 C5 1.393(6) . ?
C5 C6 1.382(7) . ?
C6 C7 1.384(7) . ?
C7 C8 1.385(7) . ?
C8 C9 1.393(7) . ?
C10 C11 1.492(6) . ?
C11 C12 1.373(7) . ?
C11 C16 1.400(6) . ?
C12 C13 1.393(7) . ?
C13 C14 1.381(7) . ?
C14 C15 1.365(7) . ?
C15 C16 1.397(6) . ?
