Synthesis, Structure, and Reactivity of Ruthenium and Osmium Nitrido Complexes with 1,2-Benzenedithiolate Ligands: N- versus S-Alkylation
Dieter Sellmann; Michael W. Wemple; Wolfgang Donaubauer; Frank W. Heinemann; Inorganic Chemistry 36 (1997) 1397–1402; doi:10.1021/ic961240b

data_4323367
_publ_contact_author
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        Dr. F. W. Heinemann                                                     
        Institut f\"ur Anorganische Chemie II                                   
        Universit\"at Erlangen-N\"urnberg                                       
        Egerlandstr. 1                                                          
        D-91058 Erlangen                                                        
        Bundesrepublik Deutschland                                              
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_publ_contact_author_email       HEINEMAN@ANORGANIK.CHEMIE.UNI-ERLANGEN.DE
_publ_contact_author_fax         '049 9131 85-7367'
_publ_contact_author_phone       '049 9131 85-7383'
_publ_section_title
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 Synthesis, Structure, and Reactivity of Ruthenium and Osmium Nitrido
 Complexes with 1,2-Benzenedithiolate Ligands: N- versus S-Alkylation
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1397
_journal_page_last               1402
_journal_paper_doi               10.1021/ic961240b
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C14 H13 Cl2 N Os S4'
_chemical_formula_weight         584.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_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            4
_cell_length_a                   8.5520(10)
_cell_length_b                   10.772(2)
_cell_length_c                   19.716(3)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      14.0
_cell_volume                     1816.3(5)
_computing_cell_refinement       'P3 (Siemens Analytical X-Ray Instr., 1989)'
_computing_data_collection       'P3 (Siemens Analytical X-Ray Instr., 1989)'
_computing_data_reduction
'XDISK (Siemens Analytical X-Ray Instr.,1989)'
_computing_molecular_graphics
;
  XP 5.03 (Siemens Analytical X-Ray Instr, 1994)
;
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'profile data from \w-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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3479
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.768
_exptl_absorpt_correction_T_max  0.145
_exptl_absorpt_correction_T_min  0.084
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.138
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.055
_refine_diff_density_min         -2.020
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(13)
_refine_ls_extinction_coef       0.0022(2)
_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_all   0.962
_refine_ls_goodness_of_fit_obs   1.020
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_restrained_S_obs      1.020
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_obs          0.0362
_refine_ls_shift/esd_max         -0.035
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0848
_refine_ls_wR_factor_obs         0.0843
_reflns_number_observed          2845
_reflns_number_total             3204
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961240b_4.cif
_cod_data_source_block           mw53
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+0.0000P] 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^)+(0.0463P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323367