#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:16:03 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179782 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/78/7007830.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_7007830
loop_
_publ_author_name
'Alegria, Elisabete C. B.'
'Martins, Luísa M D R S'
'Haukka, Matti'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Rhenium complexes of tris(pyrazolyl)methanes and sulfonate derivative.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4954
_journal_page_last               4961
_journal_paper_doi               10.1039/b611209a
_journal_year                    2006
_chemical_formula_moiety         'C16 H18 N8 O5 Re S, O4 Re'
_chemical_formula_sum            'C16 H18 N8 O9 Re2 S'
_chemical_formula_weight         870.84
_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                 100.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.500(3)
_cell_length_b                   12.532(3)
_cell_length_c                   15.166(3)
_cell_measurement_reflns_used    70279
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2337.0(9)
_computing_cell_refinement       'EvalCCD (Duisenberg, 1998-2003)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg, 1998-2003)'
_computing_molecular_graphics    'Diamond v.3.0e (Crystal Impact GbR, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_sigmaI/netI    0.0474
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28197
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    10.504
_exptl_absorpt_correction_T_max  0.4322
_exptl_absorpt_correction_T_min  0.2403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    2.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       purple
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.727
_refine_diff_density_min         -1.979
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0481
_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)+(0.0291P)²+62.7509P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                2978
_reflns_number_total             4091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b611209a.txt
_cod_data_source_block           struct_6
_cod_original_cell_volume        2337.2(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7007830
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 0.20010(5) 0.11197(5) 0.21489(3) 0.03922(18) Uani 1 1 d . . .
S1 S 0.2016(3) -0.1870(3) 0.4490(2) 0.0455(9) Uani 1 1 d . . .
O1 O 0.3118(9) -0.2240(8) 0.4677(6) 0.047(3) Uani 1 1 d . . .
N1 N 0.2990(9) 0.0835(9) 0.3412(7) 0.038(3) Uani 1 1 d . . .
C1 C 0.3764(12) 0.1405(13) 0.3871(9) 0.045(4) Uani 1 1 d . . .
H1 H 0.4082 0.2008 0.3639 0.054 Uiso 1 1 calc R . .
Re2 Re 0.38912(5) 0.43505(5) 0.22905(4) 0.0470(2) Uani 1 1 d . . .
O2 O 0.1654(9) -0.1279(9) 0.5195(6) 0.054(3) Uani 1 1 d . . .
N2 N 0.2792(10) 0.0036(10) 0.3951(7) 0.042(3) Uani 1 1 d . . .
C2 C 0.4078(14) 0.1020(13) 0.4756(11) 0.056(4) Uani 1 1 d . . .
H2 H 0.4606 0.1310 0.5224 0.067 Uiso 1 1 calc R . .
O3 O 0.1252(9) -0.2612(9) 0.4014(7) 0.055(3) Uani 1 1 d . . .
N3 N 0.0771(9) 0.0391(10) 0.2671(7) 0.042(3) Uani 1 1 d . . .
C3 C 0.3467(13) 0.0166(14) 0.4781(9) 0.051(4) Uani 1 1 d . . .
H3 H 0.3484 -0.0289 0.5285 0.062 Uiso 1 1 calc R . .
O4 O 0.2918(9) 0.3774(10) 0.1490(7) 0.059(3) Uani 1 1 d . . .
N4 N 0.0949(10) -0.0346(10) 0.3336(7) 0.043(3) Uani 1 1 d . . .
C4 C -0.0252(12) 0.0644(14) 0.2548(9) 0.051(4) Uani 1 1 d . . .
H4 H -0.0598 0.1129 0.2105 0.061 Uiso 1 1 calc R . .
O5 O 0.4863(17) 0.486(2) 0.1807(8) 0.180(13) Uani 1 1 d . . .
N5 N 0.2467(9) -0.0613(9) 0.2118(6) 0.036(3) Uani 1 1 d . . .
C5 C -0.0767(14) 0.0114(15) 0.3147(10) 0.058(4) Uani 1 1 d . . .
H5 H -0.1508 0.0170 0.3209 0.069 Uiso 1 1 calc R . .
O6 O 0.3306(14) 0.5315(13) 0.2782(13) 0.134(8) Uani 1 1 d . . .
N6 N 0.2385(8) -0.1253(8) 0.2823(6) 0.031(2) Uani 1 1 d . . .
C6 C 0.0038(12) -0.0525(14) 0.3644(10) 0.050(4) Uani 1 1 d . . .
H6 H -0.0051 -0.0999 0.4114 0.060 Uiso 1 1 calc R . .
O7 O 0.4440(11) 0.3493(12) 0.3109(11) 0.088(4) Uani 1 1 d . . .
N7 N 0.3160(9) 0.1290(10) 0.1377(7) 0.042(3) Uani 1 1 d . . .
C7 C 0.2869(11) -0.1181(12) 0.1540(9) 0.040(3) Uani 1 1 d . . .
H7 H 0.3027 -0.0922 0.0989 0.048 Uiso 1 1 calc R . .
N8 N 0.2797(10) 0.1254(11) 0.0501(8) 0.046(3) Uani 1 1 d . . .
C8 C 0.3036(11) -0.2232(12) 0.1848(9) 0.041(3) Uani 1 1 d . . .
H8 H 0.3301 -0.2816 0.1551 0.049 Uiso 1 1 calc R . .
O9 O 0.1187(8) 0.0922(9) 0.0966(6) 0.050(3) Uani 1 1 d . . .
C9 C 0.2735(11) -0.2234(12) 0.2669(8) 0.040(3) Uani 1 1 d . . .
H9 H 0.2768 -0.2828 0.3062 0.048 Uiso 1 1 calc R . .
C10 C 0.2048(11) -0.0797(11) 0.3607(8) 0.035(3) Uani 1 1 d . . .
C11 C 0.4226(11) 0.1364(12) 0.1481(10) 0.045(4) Uani 1 1 d . . .
H11 H 0.4702 0.1418 0.2043 0.054 Uiso 1 1 calc R . .
C12 C 0.4551(13) 0.1351(13) 0.0676(11) 0.053(4) Uani 1 1 d . . .
H12 H 0.5276 0.1387 0.0569 0.064 Uiso 1 1 calc R . .
C13 C 0.3645(13) 0.1279(14) 0.0065(10) 0.054(4) Uani 1 1 d . . .
H13 H 0.3603 0.1250 -0.0566 0.065 Uiso 1 1 calc R . .
C14 C 0.1610(12) 0.1249(14) 0.0210(9) 0.050(4) Uani 1 1 d . . .
C15 C 0.1285(16) 0.0450(17) -0.0545(12) 0.072(5) Uani 1 1 d . . .
H15A H 0.1441 -0.0275 -0.0315 0.109 Uiso 1 1 calc R . .
H15B H 0.1700 0.0592 -0.1023 0.109 Uiso 1 1 calc R . .
H15C H 0.0506 0.0519 -0.0783 0.109 Uiso 1 1 calc R . .
C16 C 0.1189(15) 0.2351(14) -0.0096(11) 0.060(4) Uani 1 1 d . . .
H16A H 0.0408 0.2310 -0.0336 0.090 Uiso 1 1 calc R . .
H16B H 0.1573 0.2609 -0.0563 0.090 Uiso 1 1 calc R . .
H16C H 0.1314 0.2843 0.0414 0.090 Uiso 1 1 calc R . .
O8 O 0.1769(8) 0.2329(9) 0.2481(6) 0.053(3) 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'
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'
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
O8 Re1 O9 108.3(5) . . ?
O8 Re1 N7 105.3(5) . . ?
O9 Re1 N7 77.8(4) . . ?
O8 Re1 N3 96.1(5) . . ?
O9 Re1 N3 89.7(4) . . ?
N7 Re1 N3 157.7(5) . . ?
O8 Re1 N1 89.1(5) . . ?
O9 Re1 N1 162.4(4) . . ?
N7 Re1 N1 100.2(4) . . ?
N3 Re1 N1 86.1(4) . . ?
O8 Re1 N5 163.6(4) . . ?
O9 Re1 N5 87.2(4) . . ?
N7 Re1 N5 82.8(4) . . ?
N3 Re1 N5 78.1(4) . . ?
N1 Re1 N5 75.2(4) . . ?
O3 S1 O1 114.8(7) . . ?
O3 S1 O2 116.0(7) . . ?
O1 S1 O2 116.1(6) . . ?
O3 S1 C10 101.5(6) . . ?
O1 S1 C10 103.1(6) . . ?
O2 S1 C10 102.0(6) . . ?
C1 N1 N2 106.5(12) . . ?
C1 N1 Re1 130.5(10) . . ?
N2 N1 Re1 122.4(9) . . ?
N1 C1 C2 112.0(14) . . ?
N1 C1 H1 124.0 . . ?
C2 C1 H1 124.0 . . ?
O5 Re2 O6 109.8(13) . . ?
O5 Re2 O7 109.6(9) . . ?
O6 Re2 O7 106.7(9) . . ?
O5 Re2 O4 109.4(6) . . ?
O6 Re2 O4 108.1(6) . . ?
O7 Re2 O4 113.3(7) . . ?
N1 N2 C3 108.4(12) . . ?
N1 N2 C10 120.0(11) . . ?
C3 N2 C10 131.5(12) . . ?
C3 C2 C1 103.9(14) . . ?
C3 C2 H2 128.1 . . ?
C1 C2 H2 128.1 . . ?
C4 N3 N4 107.4(11) . . ?
C4 N3 Re1 128.2(10) . . ?
N4 N3 Re1 123.6(9) . . ?
C2 C3 N2 109.2(14) . . ?
C2 C3 H3 125.4 . . ?
N2 C3 H3 125.4 . . ?
C6 N4 N3 109.9(12) . . ?
C6 N4 C10 130.9(12) . . ?
N3 N4 C10 119.2(10) . . ?
N3 C4 C5 110.7(15) . . ?
N3 C4 H4 124.7 . . ?
C5 C4 H4 124.7 . . ?
C7 N5 N6 107.5(11) . . ?
C7 N5 Re1 132.5(10) . . ?
N6 N5 Re1 119.9(7) . . ?
C4 C5 C6 104.8(14) . . ?
C4 C5 H5 127.6 . . ?
C6 C5 H5 127.6 . . ?
C9 N6 N5 109.4(10) . . ?
C9 N6 C10 131.2(11) . . ?
N5 N6 C10 119.2(10) . . ?
N4 C6 C5 107.2(13) . . ?
N4 C6 H6 126.4 . . ?
C5 C6 H6 126.4 . . ?
C11 N7 N8 106.2(11) . . ?
C11 N7 Re1 138.6(10) . . ?
N8 N7 Re1 115.0(9) . . ?
N5 C7 C8 110.1(12) . . ?
N5 C7 H7 125.0 . . ?
C8 C7 H7 125.0 . . ?
N7 N8 C13 109.5(12) . . ?
N7 N8 C14 116.5(10) . . ?
C13 N8 C14 133.9(12) . . ?
C9 C8 C7 104.9(13) . . ?
C9 C8 H8 127.5 . . ?
C7 C8 H8 127.5 . . ?
C14 O9 Re1 120.7(9) . . ?
N6 C9 C8 108.1(13) . . ?
N6 C9 H9 126.0 . . ?
C8 C9 H9 126.0 . . ?
N2 C10 N6 108.8(10) . . ?
N2 C10 N4 109.5(11) . . ?
N6 C10 N4 108.5(10) . . ?
N2 C10 S1 110.6(9) . . ?
N6 C10 S1 110.1(9) . . ?
N4 C10 S1 109.3(8) . . ?
N7 C11 C12 110.7(14) . . ?
N7 C11 H11 124.7 . . ?
C12 C11 H11 124.7 . . ?
C13 C12 C11 105.8(14) . . ?
C13 C12 H12 127.1 . . ?
C11 C12 H12 127.1 . . ?
C12 C13 N8 107.9(13) . . ?
C12 C13 H13 126.1 . . ?
N8 C13 H13 126.1 . . ?
O9 C14 N8 105.3(11) . . ?
O9 C14 C15 109.5(14) . . ?
N8 C14 C15 110.4(13) . . ?
O9 C14 C16 110.7(13) . . ?
N8 C14 C16 111.3(14) . . ?
C15 C14 C16 109.7(13) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 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
Re1 O8 1.639(11) . ?
Re1 O9 1.912(9) . ?
Re1 N7 2.031(11) . ?
Re1 N3 2.064(11) . ?
Re1 N1 2.115(12) . ?
Re1 N5 2.250(12) . ?
S1 O3 1.432(12) . ?
S1 O1 1.432(11) . ?
S1 O2 1.438(10) . ?
S1 C10 1.904(13) . ?
N1 C1 1.300(18) . ?
N1 N2 1.344(16) . ?
C1 C2 1.41(2) . ?
C1 H1 0.9500 . ?
Re2 O5 1.654(15) . ?
Re2 O6 1.657(15) . ?
Re2 O7 1.691(15) . ?
Re2 O4 1.716(11) . ?
N2 C3 1.393(18) . ?
N2 C10 1.432(18) . ?
C2 C3 1.32(2) . ?
C2 H2 0.9500 . ?
N3 C4 1.299(18) . ?
N3 N4 1.357(16) . ?
C3 H3 0.9500 . ?
N4 C6 1.325(18) . ?
N4 C10 1.474(17) . ?
C4 C5 1.38(2) . ?
C4 H4 0.9500 . ?
N5 C7 1.299(16) . ?
N5 N6 1.356(14) . ?
C5 C6 1.40(2) . ?
C5 H5 0.9500 . ?
N6 C9 1.339(18) . ?
N6 C10 1.449(15) . ?
C6 H6 0.9500 . ?
N7 C11 1.317(18) . ?
N7 N8 1.325(16) . ?
C7 C8 1.40(2) . ?
C7 H7 0.9500 . ?
N8 C13 1.347(18) . ?
N8 C14 1.470(19) . ?
C8 C9 1.363(18) . ?
C8 H8 0.9500 . ?
O9 C14 1.408(17) . ?
C9 H9 0.9500 . ?
C11 C12 1.35(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.33(2) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.52(2) . ?
C14 C16 1.52(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
