Electronic Structure of Neutral and Monoanionic Tris(benzene-1,2-dithiolato)metal Complexes of Molybdenum and Tungsten
Kapre, Ruta R.; Bothe, Eberhard; Weyhermüller, Thomas; DeBeer George, Serena; Wieghardt, Karl; Inorganic Chemistry 46 (2007) 5642–5650; doi:10.1021/ic700600r

data_4333307
_publ_section_title
;
 Electronic Structure of Neutral and Monoanionic
 Tris(benzene-1,2-dithiolato)metal Complexes of Molybdenum and Tungsten
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5642
_journal_page_last               5650
_journal_paper_doi               10.1021/ic700600r
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '[C42 H60 S6 W], 0.5 MeCN'
_chemical_formula_sum            'C43 H61.5 N0.5 S6 W'
_chemical_formula_weight         961.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.045(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7227(2)
_cell_length_b                   18.7101(4)
_cell_length_c                   23.7213(5)
_cell_measurement_temperature    100(2)
_cell_volume                     4747.18(17)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method
'1636 images at 0.9 deg. stepwise rotation in omega and phi, 18 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            90719
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    2.725
_exptl_absorpt_correction_T_max  0.8972
_exptl_absorpt_correction_T_min  0.5493
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.670
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         9679
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0177P)^2^+20.2761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                9211
_reflns_number_total             9679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700600rsup1.cif
_cod_data_source_block           3
_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 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Gaussian'
changed to 'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C43 H61.50 N0.50 S6 W'
_cod_database_code               4333307