#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:04:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179091 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/53/4305386.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_4305386
loop_
_publ_author_name
'Brenton R. Franklin'
'Richard S. Herrick'
'Christopher J. Ziegler'
'Natalie Barone'
'Laura R. Condon'
_publ_section_title
;
Reactions of the Re(CO)3(H2O)3+ Synthon with Monodentate Ligands under
Aqueous Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5902
_journal_page_last               5909
_journal_paper_doi               10.1021/ic800363w
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C15 H24 F6 O3 P Re S3'
_chemical_formula_weight         679.69
_chemical_name_systematic
;
tricarbonyltris(tetrahydrothiophene)rhenium(I) hexafluorophosphate
;
_space_group_IT_number           160
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.1729(19)
_cell_length_b                   11.1729(19)
_cell_length_c                   14.705(3)
_cell_measurement_reflns_used    4379
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.52
_cell_volume                     1589.7(5)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4443
_diffrn_reflns_theta_full        28.12
_diffrn_reflns_theta_max         28.12
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    6.171
_exptl_absorpt_correction_T_max  0.7478
_exptl_absorpt_correction_T_min  0.4407
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             990
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.015(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         969
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0169
_refine_ls_shift/su_max          0.000
_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+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0397
_refine_ls_wR_factor_ref         0.0397
_reflns_number_gt                969
_reflns_number_total             969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800363w-file002_4.cif
_cod_data_source_block           5[PF6]
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4305386
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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
C1 C 1.0804(3) 1.1608(6) 1.0209(5) 0.0219(14) Uani 1 2 d S . .
C2 C 0.9303(8) 0.6607(10) 0.8863(6) 0.0152(15) Uani 0.50 1 d P A 1
C3 C 0.9759(8) 0.7054(8) 0.8306(5) 0.0153(14) Uani 0.50 1 d P A 2
C4 C 0.8972(8) 0.5800(10) 0.8928(5) 0.0185(15) Uani 0.50 1 d P A 2
C5 C 0.7961(3) 0.5923(5) 0.9500(3) 0.0162(10) Uani 1 2 d S . 2
F1 F 0.26571(17) 0.73429(17) 0.9008(2) 0.0337(8) Uani 1 2 d S . .
F2 F 0.4015(2) 0.5985(2) 1.0252(3) 0.0501(11) Uani 1 2 d S . .
O1 O 1.1287(3) 1.2575(5) 1.0638(3) 0.0466(17) Uani 1 2 d S . .
P1 P 0.3333 0.6667 0.96355(17) 0.0171(5) Uani 1 6 d S . .
Re1 Re 1.0000 1.0000 0.943620(13) 0.00802(8) Uani 1 6 d S . .
S1 S 0.90134(10) 0.8027(2) 0.83361(12) 0.0327(5) Uani 1 2 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.035(3) 0.008(3) 0.013(3) 0.000(2) 0.0002(11) 0.0040(15)
C2 0.012(4) 0.010(4) 0.025(5) 0.004(3) 0.002(3) 0.007(3)
C3 0.017(3) 0.014(3) 0.022(4) 0.005(3) 0.003(3) 0.013(3)
C4 0.015(4) 0.024(5) 0.022(4) 0.007(3) 0.003(3) 0.013(4)
C5 0.0175(19) 0.014(2) 0.016(2) 0.0014(18) 0.0007(9) 0.0068(12)
F1 0.0301(14) 0.0301(14) 0.047(2) 0.0074(8) -0.0074(8) 0.0195(16)
F2 0.058(2) 0.058(2) 0.045(2) 0.0139(10) -0.0139(10) 0.038(2)
O1 0.087(4) 0.012(3) 0.017(2) -0.008(2) -0.0041(11) 0.0058(13)
P1 0.0157(7) 0.0157(7) 0.0198(12) 0.000 0.000 0.0079(3)
Re1 0.00794(10) 0.00794(10) 0.00819(13) 0.000 0.000 0.00397(5)
S1 0.0624(10) 0.0063(9) 0.0107(9) -0.0021(7) -0.0010(4) 0.0031(5)
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'
F F 0.0171 0.0103 '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'
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 C1 Re1 177.9(6) . . ?
C4 C3 S1 109.6(5) . . ?
C5 C4 C3 111.9(7) . . ?
C4 C5 C4 109.3(7) . 5_655 ?
F1 P1 F1 90.1(2) . 2_665 ?
F1 P1 F1 90.1(2) . 3_565 ?
F1 P1 F1 90.1(2) 2_665 3_565 ?
F1 P1 F2 89.40(14) . 2_665 ?
F1 P1 F2 179.3(3) 2_665 2_665 ?
F1 P1 F2 89.40(14) 3_565 2_665 ?
F1 P1 F2 89.40(14) . 3_565 ?
F1 P1 F2 89.40(14) 2_665 3_565 ?
F1 P1 F2 179.3(3) 3_565 3_565 ?
F2 P1 F2 91.1(3) 2_665 3_565 ?
F1 P1 F2 179.3(3) . . ?
F1 P1 F2 89.40(14) 2_665 . ?
F1 P1 F2 89.40(14) 3_565 . ?
F2 P1 F2 91.1(3) 2_665 . ?
F2 P1 F2 91.1(3) 3_565 . ?
C1 Re1 C1 88.8(3) . 3_675 ?
C1 Re1 C1 88.8(3) . 2_765 ?
C1 Re1 C1 88.8(3) 3_675 2_765 ?
C1 Re1 S1 175.9(2) . . ?
C1 Re1 S1 94.19(14) 3_675 . ?
C1 Re1 S1 94.19(14) 2_765 . ?
C1 Re1 S1 94.19(14) . 3_675 ?
C1 Re1 S1 175.9(2) 3_675 3_675 ?
C1 Re1 S1 94.19(14) 2_765 3_675 ?
S1 Re1 S1 82.71(6) . 3_675 ?
C1 Re1 S1 94.19(14) . 2_765 ?
C1 Re1 S1 94.19(14) 3_675 2_765 ?
C1 Re1 S1 175.9(2) 2_765 2_765 ?
S1 Re1 S1 82.71(6) . 2_765 ?
S1 Re1 S1 82.71(6) 3_675 2_765 ?
C3 S1 C3 111.2(5) 5_655 . ?
C3 S1 C2 29.8(3) 5_655 5_655 ?
C3 S1 C2 95.0(4) . 5_655 ?
C3 S1 C2 95.0(4) 5_655 . ?
C3 S1 C2 29.8(3) . . ?
C2 S1 C2 70.6(5) 5_655 . ?
C3 S1 Re1 116.6(3) 5_655 . ?
C3 S1 Re1 116.6(3) . . ?
C2 S1 Re1 106.5(2) 5_655 . ?
C2 S1 Re1 106.5(2) . . ?
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
C1 O1 1.129(7) . ?
C1 Re1 1.927(7) . ?
C2 S1 1.933(9) . ?
C3 C4 1.530(10) . ?
C3 S1 1.668(7) . ?
C4 C5 1.469(8) . ?
C5 C4 1.469(8) 5_655 ?
F1 P1 1.601(3) . ?
F2 P1 1.602(4) . ?
P1 F1 1.601(3) 2_665 ?
P1 F1 1.601(3) 3_565 ?
P1 F2 1.602(4) 2_665 ?
P1 F2 1.602(4) 3_565 ?
Re1 C1 1.927(7) 3_675 ?
Re1 C1 1.927(7) 2_765 ?
Re1 S1 2.502(2) . ?
Re1 S1 2.502(2) 3_675 ?
Re1 S1 2.502(2) 2_765 ?
S1 C3 1.668(7) 5_655 ?
S1 C2 1.933(9) 5_655 ?
