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_7009028
_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     ' Ru(II) (Cl 1-)3 ((CH3)2SO)2 (NH2NH3 1+)'
_chemical_formula_sum            'C4 H17 Cl3 N2 O2 Ru S2'
_chemical_formula_weight         396.74
_chemical_name_systematic
;
 mer-cis-trichloro dis(dimethylsulfoxide) hydrazinium ruthenium(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.55(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.202(4)
_cell_length_b                   8.455(1)
_cell_length_c                   12.918(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     2743.3(7)
_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_measured_fraction_theta_full 0.470
_diffrn_measured_fraction_theta_max 0.470
_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  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4155
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0.2
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.012
_exptl_absorpt_correction_T_max  100.00
_exptl_absorpt_correction_T_min  69.74
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.90
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.00118(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         3985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+2.4581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                3781
_reflns_number_total             3985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908170d.txt
_cod_data_source_block           3
_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^)+(0.0426P)^2^+2.4581P] 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^)+(0.0426P)^2^+2.4581P] 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      C2/c
_cod_database_code               7009028