Transition Metal Complexes with Sulfur Ligands. 136.1 Enforced Trans Coordination of Thiolate Donors in Electron Rich Iron, Ruthenium, and Nickel [M(L)(pyN~2~H~2~S~2~)] and [M(L)(pyS~4~)] Complexes (L = CO, PPh~3~, DMSO) (pyN2H2S22-= 2,6-Bis(2-mercaptophenylamino)dimethylpyridine(2-); pyS4^2-^ = 2,6-Bis(2-mercaptophenylthio)dimethylpyridine(2-))
Dieter Sellmann; Jürgen Utz; Frank W. Heinemann; Inorganic Chemistry 38 (1999) 5314–5322; doi:10.1021/ic990169h

data_4322369
_publ_contact_author
;
        Prof. Dr. D. Sellmann
        Institut f\"ur Anorganische Chemie II
        Universit\"at Erlangen-N\"urnberg
        Egerlandstr. 1
        D-91058 Erlangen
        Bundesrepublik Deutschland
;
_publ_contact_author_email       SELLMANN@ANORGANIK.CHEMIE.UNI-ERLANGEN.DE
_publ_contact_author_fax         '049 9131 852-7367'
_publ_contact_author_phone       '049 9131 852-7360'
_publ_section_title
;
 Transition Metal Complexes with Sulfur Ligands. 136.1 Enforced Trans
 Coordination of Thiolate Donors in Electron Rich Iron, Ruthenium, and
 Nickel [M(L)(pyN~2~H~2~S~2~)] and [M(L)(pyS~4~)] Complexes (L = CO,
 PPh~3~, DMSO) (pyN2H2S22-=
 2,6-Bis(2-mercaptophenylamino)dimethylpyridine(2-); pyS4^2-^ =
 2,6-Bis(2-mercaptophenylthio)dimethylpyridine(2-))
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5314
_journal_page_last               5322
_journal_paper_doi               10.1021/ic990169h
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C21 H19 Fe N O2 S4'
_chemical_formula_weight         501.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                67.97(4)
_cell_angle_beta                 84.30(3)
_cell_angle_gamma                88.50(4)
_cell_formula_units_Z            2
_cell_length_a                   8.405(3)
_cell_length_b                   11.260(6)
_cell_length_c                   12.265(5)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.6
_cell_measurement_theta_min      12.3
_cell_volume                     1070.6(9)
_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
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_publication_material
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_structure_refinement
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_structure_solution
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nicolet R3m/V'
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5365
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         2.10
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.113
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       column
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.923
_refine_ls_goodness_of_fit_obs   1.035
_refine_ls_hydrogen_treatment    'refall except H2 noref'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_restrained_S_obs      1.035
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_obs          0.0268
_refine_ls_shift/esd_max         0.098
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0686
_refine_ls_wR_factor_obs         0.0662
_reflns_number_observed          3595
_reflns_number_total             4737
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990169h_1.cif
_cod_data_source_block           ju40
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0419P)^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^)+(0.0419P)^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 
;
_cod_original_cell_volume        1070.6(8)
_cod_database_code               4322369