Unusual pathways for the reaction between [MCl2(Me2SO)4] (M = Os, Ru) and hydrazine dihydrochloride: deoxygenation of sulfoxides vs. coordination of hydrazinium
da Silva, M. Fátima C. Guedes; Pombeiro, Armando J. L.; Geremia, Silvano; Zangrando, Ennio; Calligaris, Mario; Zinchenko, Andrey V.; Kukushkin, Vadim Yu.; Journal of the Chemical Society, Dalton Transactions  (2000) 1363–; doi:10.1039/a908170d

data_7009026
_publ_section_title
;
 Unusual pathways for the reaction between [MCl2(Me2SO)4]
 (M&#x2005;=&#x2005;Os, Ru) and hydrazine dihydrochloride:
 deoxygenation of sulfoxides vs. coordination of hydrazinium
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1363
_journal_paper_doi               10.1039/a908170d
_journal_year                    2000
_chemical_formula_structural     'Os(III) (Cl 1-)3 (NH3)2 S(CH3)2 '
_chemical_formula_sum            'C2 H12 Cl3 N2 Os S'
_chemical_formula_weight         392.75
_chemical_name_systematic
;
 mer-cis-trichloro diammine dimethylsulfide osmium(III)
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5765(10)
_cell_length_b                   8.9186(8)
_cell_length_c                   11.8001(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      13
_cell_volume                     994.22(16)
_computing_cell_refinement       'CELDIM (Enraf Nonius)'
_computing_data_collection       'CAD4 package (Enraf Nonius)'
_computing_data_reduction        'local program'
_computing_molecular_graphics
;
locally modified version of ORTEP (Johnson, 1965; Mallinson & Muir, 1985)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       'w/2\q 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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2896
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.774
_exptl_absorpt_correction_T_max  100.0
_exptl_absorpt_correction_T_min  29.24
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    2.624
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.259
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.059
_refine_ls_goodness_of_fit_obs   1.099
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         2896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.099
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_obs          0.0291
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+2.0582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0787
_refine_ls_wR_factor_obs         0.0771
_reflns_number_observed          2594
_reflns_number_total             2896
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908170d.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'psi scan' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+2.0582P] 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^)+(0.0510P)^2^+2.0582P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        994.2(2)
_cod_original_sg_symbol_H-M      'P 21/c (N.14)'
_cod_database_code               7009026
_diffrn_standards_decay_corr_max 1.106
_diffrn_standards_decay_corr_min 0.997