Molybdenum complexes with tridentate NS2 ligands. Synthesis, crystal structures and spectroscopic properties
Stelzig, Lutz; Kötte, Stephan; Krebs, Bernt; Journal of the Chemical Society, Dalton Transactions  (1998) 2921–; doi:10.1039/a802334d

data_7028004
_publ_section_title
;
 Molybdenum complexes with tridentate NS2 ligands. Synthesis, crystal
 structures and spectroscopic properties
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2921
_journal_paper_doi               10.1039/a802334d
_journal_year                    1998
_chemical_formula_sum            'C57 H48 Cl6 Mo2 N6 O3 S4'
_chemical_formula_weight         1397.83
_chemical_name_common
;
(2-oxo)Bis(1-mercaptobenzaldehyde)
-4-triphenylmethylthiosemicarbazone-S,S,N)-oxo-molybdenum(V) 
;
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 121.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.449(4)
_cell_length_b                   19.763(4)
_cell_length_c                   18.450(4)
_cell_measurement_temperature    293(2)
_cell_volume                     6041(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0892
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24807
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         5.30
_exptl_absorpt_coefficient_mu    0.867
_exptl_crystal_colour            'deep red to violet'
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.686
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0039(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.080
_refine_ls_goodness_of_fit_obs   1.036
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_restrained_S_obs      1.036
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_obs          0.0672
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+19.4345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2131
_refine_ls_wR_factor_obs         0.1657
_reflns_number_observed          4575
_reflns_number_total             6700
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            D802334sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+19.4345P] 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^)+(0.0889P)^2^+19.4345P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6040.8(22)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7028004