Synthesis, Structures, and Properties of 1,2,4,5-Benzenetetrathiolate Linked Group 10 Metal Complexes
Kuppuswamy Arumugam; Mohamed C. Shaw; P. Chandrasekaran; Dino Villagrán; Thomas G. Gray; Joel T. Mague; James P. Donahue; Inorganic Chemistry 48 (2009) 10591–10607; doi:10.1021/ic901257s

data_4303581
_publ_contact_author             'James P. Donahue'
_publ_contact_author_address
;
   James P. Donahue
   Department of Chemistry
   Tulane University
   Percival Stern Hall, Room 2015
   6400 Freret Street
   New Orleans, Louisiana 70118-5698
;
_publ_contact_author_email       donahue@tulane.edu
_publ_section_title
;
Synthesis, Structures, and Properties of 1,2,4,5-Benzenetetrathiolate
Linked Group 10 Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10591
_journal_page_last               10607
_journal_paper_doi               10.1021/ic901257s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '(C40 H68 Ni P2 S4 Sn), 0.5(C2 H4 Cl2)'
_chemical_formula_sum            'C41 H70 Cl Ni P2 S4 Sn'
_chemical_formula_weight         966.07
_chemical_name_systematic
; 
 Di-n-butyltin(\m-1,2,4,5-tetrathiolatobenzene)(1,2-bis(di 
 cyclohexylphosphino)ethane)nickel(II) 1,2-dichloroethane 
 hemisolvate 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.497(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   38.367(3)
_cell_length_b                   10.3214(9)
_cell_length_c                   48.842(4)
_cell_measurement_reflns_used    9624
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.31
_cell_volume                     19176(3)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2008a)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2008a)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008b)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            155239
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  0.9239
_exptl_absorpt_correction_T_min  0.8199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Column
_exptl_crystal_F_000             8080
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
;
_refine_diff_density_max         2.379
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1822
_refine_ls_number_reflns         34626
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+211.6400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.1795
_reflns_number_gt                25356
_reflns_number_total             34626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901257s_si_001_16.cif
_cod_data_source_block           jpd246a1_0m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_database_code               4303581