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_7009027
_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_moiety         'Os(II) (Cl 1-)2 ((CH3)2SO)4'
_chemical_formula_sum            'C8 H24 Cl2 O4 Os S4'
_chemical_formula_weight         573.61
_chemical_name_systematic
;
 trans dichloro tetrakis(dimethylsulfoxide) osmium(II)
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.0951(7)
_cell_length_b                   9.0951(7)
_cell_length_c                   11.1941(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     925.99(16)
_computing_cell_refinement       'CELDIM (Enraf Nonius) '
_computing_data_collection       'CAD4 package (Enraf Nonius)'
_computing_data_reduction        'local program'
_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  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0156
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            786
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         2.89
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.629
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.126
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         708
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.125
_refine_ls_restrained_S_obs      1.125
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_obs          0.0163
_refine_ls_shift/esd_max         0.045
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+0.4271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0433
_refine_ls_wR_factor_obs         0.0433
_reflns_number_observed          708
_reflns_number_total             708
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908170d.txt
_cod_data_source_block           1
_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^)+(0.0283P)^2^+0.4271P] 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^)+(0.0283P)^2^+0.4271P] 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        926.0(2)
_cod_database_code               7009027
_diffrn_standards_decay_corr_max 1.063
_diffrn_standards_decay_corr_min 0.999