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_4333309
_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
'[C16 H36]+, [C42 H60 N S6 W]-, 0.19 (C H2 Cl2)'
_chemical_formula_sum            'C58.19 H96.38 Cl0.38 N S6 W'
_chemical_formula_weight         1199.49
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.68(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5159(8)
_cell_length_b                   21.949(2)
_cell_length_c                   20.174(2)
_cell_measurement_temperature    100(2)
_cell_volume                     6424.9(9)
_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 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method
'606 images at 0.5 deg. stepwise rotation in omega and phi, 72 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  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0762
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28186
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    2.042
_exptl_absorpt_correction_T_max  0.9591
_exptl_absorpt_correction_T_min  0.8921
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         8319
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+27.6408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                6060
_reflns_number_total             8319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700600rsup1.cif
_cod_data_source_block           5
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+27.6408P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+27.6408P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P2(1)/c '
_cod_database_code               4333309