Necessity of fine tuning in Mo(iv) bis(dithiolene) complexes to warrant nitrate reduction
Majumdar, Amit; Pal, Kuntal; Sarkar, Sabyasachi; Dalton Transactions  (2009) 1927–1938; doi:10.1039/b815436h

data_7000725
_publ_section_title
;
 Necessity of fine tuning in Mo(iv) bis(dithiolene) complexes to
 warrant nitrate reduction
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              1927
_journal_page_last               1938
_journal_paper_doi               10.1039/b815436h
_journal_year                    2009
_chemical_compound_source        'Sodium Molybdate'
_chemical_formula_moiety         'C33 H22 Mo N4 P S5 , C8 H20 N, C H2 Cl2'
_chemical_formula_sum            'C42 H44 Cl2 Mo N5 P S5'
_chemical_formula_weight         976.98
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                100.126(5)
_cell_angle_beta                 101.684(5)
_cell_angle_gamma                97.983(5)
_cell_formula_units_Z            2
_cell_length_a                   11.086(5)
_cell_length_b                   11.646(5)
_cell_length_c                   18.305(5)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.32
_cell_volume                     2240.7(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      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14920
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.9722
_exptl_absorpt_correction_T_min  0.9442
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Violet
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             988
_exptl_crystal_recrystallization_method 'Dichloromethane, petroleum ether'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         10640
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+23.5508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.2109
_reflns_number_gt                7697
_reflns_number_total             10640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815436h.txt
_cod_data_source_block           13apram
_cod_database_code               7000725