#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:37:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179799 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/95/7009515.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_7009515
loop_
_publ_author_name
'Friebe, Matthias'
'Spies, Hartmut'
'Seichter, Wilhelm'
'Leibnitz, Peter'
'Johannsen, Bernd'
_publ_section_title
;
 Neutral '3 + 1' mixed-ligand oxorhenium(V) complexes
 with tridentate [S,N,S] chelates and aminoalkanethiols: synthesis,
 characterization and structure determination ‡
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2471
_journal_paper_doi               10.1039/b001600o
_journal_year                    2000
_chemical_formula_sum            'C11 H23 N2 O2 Re S3'
_chemical_formula_weight         497.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 111.11(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.767(3)
_cell_length_b                   11.422(9)
_cell_length_c                   13.299(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      12.177
_cell_measurement_theta_min      7.847
_cell_volume                     1667.5(16)
_computing_cell_refinement       'Enraf-Nonius CAD4H'
_computing_data_collection       'Enraf-Nonius CAD4H'
_computing_data_reduction        'Enraf-Nonius START'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega-2theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.4238
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3441
_diffrn_reflns_theta_full        26.07
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        1.78
_diffrn_standards_interval_time  180
_exptl_absorpt_coefficient_mu    7.662
_exptl_absorpt_correction_T_max  37.41
_exptl_absorpt_correction_T_min  19.33
_exptl_absorpt_correction_type   'semi empirical using psi scans'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.825
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.233
_refine_ls_extinction_coef       0.0023(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.286
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.080
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0958P)²+7.3781P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1725
_reflns_number_gt                2534
_reflns_number_total             3279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001600o.txt
_cod_data_source_block           FRIEBE1e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0958P)^2^+7.3781P] 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^)+(0.0958P)^2^+7.3781P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/N
_cod_database_code               7009515
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re Re 0.79766(4) 0.16822(4) 0.68275(3) 0.0444(2) Uani 1 d . . .
S1 S 0.9047(3) 0.0689(3) 0.5959(2) 0.0585(8) Uani 1 d . . .
S2 S 0.6304(3) 0.0594(3) 0.5930(3) 0.0611(8) Uani 1 d . . .
S3 S 0.9563(4) 0.1112(5) 0.8323(3) 0.0872(13) Uani 1 d . . .
O1 O 0.7975(10) 0.3080(9) 0.6477(8) 0.072(3) Uani 1 d . . .
O2 O 0.6366(9) 0.0838(8) 0.0455(7) 0.069(2) Uani 1 d . . .
N1 N 0.7082(10) 0.1849(10) 0.7976(10) 0.062(3) Uani 1 d . . .
N2 N 0.7023(8) 0.0886(8) 0.2720(7) 0.048(2) Uani 1 d . . .
C1 C 0.6245(15) 0.0872(13) 0.7927(13) 0.074(4) Uani 1 d . . .
H1A H 0.5785 0.1041 0.8386 0.102(14) Uiso 1 calc R . .
H1B H 0.6708 0.0161 0.8186 0.102(14) Uiso 1 calc R . .
C2 C 0.5385(13) 0.0700(19) 0.6785(12) 0.087(5) Uani 1 d . . .
H2A H 0.4827 0.1356 0.6560 0.102(14) Uiso 1 calc R . .
H2B H 0.4914 -0.0010 0.6729 0.102(14) Uiso 1 calc R . .
C3 C 0.918(3) 0.174(3) 0.940(2) 0.064(7) Uiso 0.50 d P A 1
H3A H 0.9330 0.1163 0.9975 0.102(14) Uiso 0.50 calc PR A 1
H3B H 0.9700 0.2406 0.9698 0.102(14) Uiso 0.50 calc PR A 1
C4 C 0.7921(18) 0.211(2) 0.9060(13) 0.103(6) Uani 1 d . . .
H4A H 0.7921 0.2949 0.9153 0.102(14) Uiso 1 calc R B 1
H4B H 0.7580 0.1768 0.9558 0.102(14) Uiso 1 calc R B 1
C5 C 0.8118(12) 0.0252(11) 0.4608(10) 0.057(3) Uani 1 d . . .
H5A H 0.8558 -0.0330 0.4359 0.102(14) Uiso 1 calc R . .
H5B H 0.7381 -0.0115 0.4625 0.102(14) Uiso 1 calc R . .
C6 C 0.7774(11) 0.1236(12) 0.3823(10) 0.058(3) Uani 1 d . . .
H6A H 0.7331 0.1815 0.4071 0.102(14) Uiso 1 calc R . .
H6B H 0.8511 0.1605 0.3811 0.102(14) Uiso 1 calc R . .
C7 C 0.6497(14) 0.1881(12) 0.2065(11) 0.066(4) Uani 1 d . . .
H7A H 0.7136 0.2379 0.2002 0.102(14) Uiso 1 calc R . .
H7B H 0.6027 0.2333 0.2395 0.102(14) Uiso 1 calc R . .
C8 C 0.5680(14) 0.1472(14) 0.0960(10) 0.072(4) Uani 1 d . . .
H8A H 0.5041 0.0977 0.1025 0.102(14) Uiso 1 calc R . .
H8B H 0.5300 0.2143 0.0520 0.102(14) Uiso 1 calc R . .
C9 C 0.6946(12) -0.0142(13) 0.1109(10) 0.064(3) Uani 1 d . . .
H9A H 0.7425 -0.0564 0.0767 0.102(14) Uiso 1 calc R . .
H9B H 0.6331 -0.0671 0.1174 0.102(14) Uiso 1 calc R . .
C10 C 0.7749(10) 0.0246(11) 0.2198(9) 0.054(3) Uani 1 d . . .
H10A H 0.8132 -0.0429 0.2631 0.102(14) Uiso 1 calc R . .
H10B H 0.8385 0.0750 0.2140 0.102(14) Uiso 1 calc R . .
C11 C 0.628(3) 0.296(2) 0.768(2) 0.140(10) Uani 1 d . . .
H11A H 0.5804 0.2955 0.6926 0.11(4) Uiso 1 calc R . .
H11B H 0.6785 0.3641 0.7861 0.11(4) Uiso 1 calc R . .
H11C H 0.5740 0.2964 0.8084 0.11(4) Uiso 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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
O1 Re N1 99.3(5) . . ?
O1 Re S2 117.7(4) . . ?
N1 Re S2 82.4(3) . . ?
O1 Re S3 115.9(4) . . ?
N1 Re S3 82.1(3) . . ?
S2 Re S3 125.82(18) . . ?
O1 Re S1 106.2(4) . . ?
N1 Re S1 154.0(3) . . ?
S2 Re S1 89.65(12) . . ?
S3 Re S1 82.65(13) . . ?
C5 S1 Re 113.1(4) . . ?
C2 S2 Re 103.3(5) . . ?
C3 S3 C31 21.8(12) . . ?
C3 S3 Re 102.7(10) . . ?
C31 S3 Re 101.5(10) . . ?
C8 O2 C9 109.9(10) . . ?
C4 N1 C1 113.7(14) . . ?
C4 N1 C11 102.7(16) . . ?
C1 N1 C11 105.6(16) . . ?
C4 N1 Re 113.0(9) . . ?
C1 N1 Re 113.0(8) . . ?
C11 N1 Re 107.8(12) . . ?
C7 N2 C6 111.4(10) . . ?
C7 N2 C10 107.7(10) . . ?
C6 N2 C10 111.3(9) . . ?
N1 C1 C2 109.9(12) . . ?
N1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C1 C2 S2 107.6(9) . . ?
C1 C2 H2A 110.2 . . ?
S2 C2 H2A 110.2 . . ?
C1 C2 H2B 110.2 . . ?
S2 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
C4 C3 S3 113(2) . . ?
C4 C3 H3A 109.1 . . ?
S3 C3 H3A 109.1 . . ?
C4 C3 H3B 109.0 . . ?
S3 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 N1 120.5(19) . . ?
C3 C4 H4A 107.3 . . ?
N1 C4 H4A 107.2 . . ?
C3 C4 H4B 107.1 . . ?
N1 C4 H4B 107.2 . . ?
H4A C4 H4B 106.8 . . ?
C6 C5 S1 113.8(9) . . ?
C6 C5 H5A 108.8 . . ?
S1 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
S1 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
N2 C6 C5 114.1(11) . . ?
N2 C6 H6A 108.7 . . ?
C5 C6 H6A 108.7 . . ?
N2 C6 H6B 108.7 . . ?
C5 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
N2 C7 C8 109.3(11) . . ?
N2 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
N2 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.3 . . ?
O2 C8 C7 110.3(12) . . ?
O2 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
O2 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
O2 C9 C10 110.9(11) . . ?
O2 C9 H9A 109.5 . . ?
C10 C9 H9A 109.5 . . ?
O2 C9 H9B 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
N2 C10 C9 109.5(9) . . ?
N2 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
N2 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
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
Re O1 1.663(10) . ?
Re N1 2.153(12) . ?
Re S2 2.270(3) . ?
Re S3 2.278(4) . ?
Re S1 2.293(3) . ?
S1 C5 1.805(13) . ?
S2 C2 1.834(15) . ?
S3 C3 1.81(3) . ?
S3 C31 1.83(3) . ?
O2 C8 1.420(17) . ?
O2 C9 1.431(16) . ?
N1 C4 1.454(19) . ?
N1 C1 1.474(17) . ?
N1 C11 1.54(3) . ?
N2 C7 1.431(16) . ?
N2 C6 1.469(14) . ?
N2 C10 1.475(15) . ?
C1 C2 1.50(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.44(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.487(18) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.511(19) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.483(17) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
