Mono-oxo Bis(dithiolene) Mo(IV)/W(IV) Complexes as Building Blocks for Sulfide Bridged Bi- and Tri-Nuclear Complexes
Amit Majumdar; Joyee Mitra; Kuntal Pal; Sabyasachi Sarkar; Inorganic Chemistry 47 (2008) 5360–5364; doi:10.1021/ic800466x

data_4305131
_publ_contact_author_address
;Department of Chemistry
IIT Kanpur
Kanpur -  208016
India 
;
_publ_contact_author_email       abya@iitk.ac.in
_publ_contact_author_fax         91-512-2597265
_publ_contact_author_name        'Sabyasachi Sarkar'
_publ_contact_author_phone       91-512-2597386
_publ_section_title
;
Mono-oxo Bis(dithiolene) Mo(IV)/W(IV) Complexes as Building Blocks for
Sulfide Bridged Bi- and Tri-Nuclear Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5360
_journal_page_last               5364
_journal_paper_doi               10.1021/ic800466x
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C36 H30 N P2, 0.5(C16 N8 S10 W2)'
_chemical_formula_sum            'C44 H30 N5 P2 S5 W'
_chemical_formula_weight         1034.86
_chemical_name_systematic        '[PNP]2[W2(S)2(mnt)4]'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.992(5)
_cell_angle_beta                 101.490(5)
_cell_angle_gamma                101.887(5)
_cell_formula_units_Z            2
_cell_length_a                   9.596(5)
_cell_length_b                   14.382(5)
_cell_length_c                   16.810(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2192.4(15)
_computing_cell_refinement       'SAINT 6.45(Bruker, 2003)'
_computing_data_collection       'SMART 5.628(Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45(Bruker, 2003)'
_computing_molecular_graphics    'Diamond 2.1e, ORTEP'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.1127
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14489
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    2.983
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1026
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         10387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1079P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.2224
_reflns_number_gt                6532
_reflns_number_total             10387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800466x-file003_2.cif
_cod_data_source_block           21febdm
_cod_database_code               4305131