Transition-Metal Complexes with Sulfur Ligands. 132.1 Electron-Rich Fe and Ru Complexes with [MN~2~S~3~] Cores Containing the New Pentadentate Ligand 'N~2~H~2~S~3~'^2-^ (= 2,2'-Bis(2-mercaptophenylamino)diethyl Sulfide(2-))
Dieter Sellmann; Jürgen Utz; Frank W. Heinemann; Inorganic Chemistry 38 (1999) 459–466; doi:10.1021/ic980383q

data_4321755
_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 85-7367'
_publ_contact_author_phone       '049 9131 85-7360'
_publ_section_title
;
 Transition-Metal Complexes with Sulfur Ligands. 132.1 Electron-Rich Fe
 and Ru Complexes with [MN~2~S~3~] Cores Containing the New Pentadentate
 Ligand 'N~2~H~2~S~3~'^2-^ (= 2,2'-Bis(2-mercaptophenylamino)diethyl
 Sulfide(2-))
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              459
_journal_page_last               466
_journal_paper_doi               10.1021/ic980383q
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C33 H55 N2 O2 P Ru S3'
_chemical_formula_weight         740.01
_chemical_name_systematic
; 
 ? 
;
_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   'difmap except THF geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.35(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.537(3)
_cell_length_b                   24.437(7)
_cell_length_c                   14.531(7)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      12.4
_cell_volume                     3655(2)
_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
'SHELXTL PLUS 4.21/V (Siemens An. X-Ray Instr., 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  0.0742
_diffrn_reflns_av_sigmaI/netI    0.1500
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12031
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         2.15
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.675
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.716
_refine_ls_goodness_of_fit_obs   0.984
_refine_ls_hydrogen_treatment    'refall except THF'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         8036
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.728
_refine_ls_restrained_S_obs      1.001
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_obs          0.0429
_refine_ls_shift/esd_max         12.135
_refine_ls_shift/esd_mean        0.510
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0889
_refine_ls_wR_factor_obs         0.0823
_reflns_number_observed          3914
_reflns_number_total             8036
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980383q_4.cif
_cod_data_source_block           ju37
_cod_original_cell_volume        3655.0(23)
_cod_database_code               4321755