Heteropolymetallic complexes containing ReO4-: Catalytic oxidation of sulfide
Chen Li; Xiao Peng; Shou-Chun Zhang; Li-Yuan Chai; Xiao-Yi Yi; Inorganica Chimica Acta 398 (2013) 113–116; doi:

data_1516819
_publ_section_title
;
 Heteropolymetallic complexes containing ReO4-: Catalytic oxidation of
 sulfide
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              113
_journal_page_last               116
_journal_volume                  398
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C72 H104 N4 O13 Re2 Ti2, 2(C4 H10 O)'
_chemical_formula_sum            'C80 H124 N4 O15 Re2 Ti2'
_chemical_formula_weight         1850.03
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.6520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.90220(10)
_cell_length_b                   17.85220(10)
_cell_length_c                   24.90960(10)
_cell_measurement_reflns_used    34679
_cell_measurement_temperature    133
_cell_measurement_theta_max      71.4046
_cell_measurement_theta_min      2.8555
_cell_volume                     8849.76(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'smtbx-flip (Bourhis, 2008)'
_diffrn_ambient_temperature      133
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
1 omega   44.00  144.80   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000  117.0000 126

2 omega -107.00  -67.80   0.8000   14.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000  179.0000   90.0000 49

3 omega -140.00  -68.00   0.8000   14.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000  179.0000 -180.0000 90

4 omega  -26.00   30.00   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -77.0000  -90.0000 70

5 omega   29.00  126.60   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000   38.0000 -180.0000 122

6 omega   77.00  125.00   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000   90.0000 60

7 omega   43.00   71.00   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000   30.0000 35

8 omega   88.00  148.80   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000 -101.0000 76

9 omega   37.00   70.60   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -90.0000 42

10 omega   39.00   68.60   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000 -150.0000 37

11 omega   39.00   67.80   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  120.0000 36

12 omega   40.00   77.60   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000 -171.0000 47

13 omega   37.00   70.60   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000   60.0000 42

14 omega  103.00  164.60   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000    0.0000   90.0000 77

15 omega   43.00   72.60   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000 -101.0000 37

16 omega   39.00   68.60   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000 -180.0000 37

17 omega   48.00  100.00   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000    0.0000   90.0000 65

18 omega   41.00   69.80   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -60.0000 36

19 omega   38.00   71.60   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  150.0000 42

20 omega   40.00   68.00   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000   30.0000 35

21 omega   93.00  149.00   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000 -171.0000 70

22 omega   41.00   69.80   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -30.0000 36

23 omega   40.00   77.60   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000    0.0000 47

24 omega   88.00  176.00   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   50.0000  -60.0000 110

25 omega   53.00   77.80   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000   90.0000 31

26 omega   79.00  135.00   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000   -9.0000 70

27 omega   40.00   67.20   0.8000   18.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000   -9.0000 34

28 omega  -12.00   84.00   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  -77.0000   30.0000 120

29 omega   41.00  125.00   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000   38.0000  -90.0000 105

30 omega  -70.00  -30.80   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -77.0000  -90.0000 49
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      0.0571636
_diffrn_orient_matrix_UB_12      -0.0314419
_diffrn_orient_matrix_UB_13      -0.0345962
_diffrn_orient_matrix_UB_21      0.0521434
_diffrn_orient_matrix_UB_22      0.0335383
_diffrn_orient_matrix_UB_23      0.039331
_diffrn_orient_matrix_UB_31      -0.0005571
_diffrn_orient_matrix_UB_32      -0.0730809
_diffrn_orient_matrix_UB_33      0.0328855
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58968
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_exptl_absorpt_coefficient_mu    7.174
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.24987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.955
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1879
_refine_ls_number_reflns         26226
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0359
_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/[\s^2^(Fo^2^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                24129
_reflns_number_total             26226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-398-113-116.cif
_cod_data_source_block           YXY239A
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               1516819