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_7028003
_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            'C31 H33 Mo N3 O5 S2'
_chemical_formula_weight         687.66
_chemical_name_common
;
cis-Dioxo-1(1-(2-mercapto-acetophenone)-4-triphenylmethylthiosemicarbazone
-S,S,N))(methanol)molybdenum(VI) 
;
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                75.660(10)
_cell_angle_beta                 83.290(10)
_cell_angle_gamma                64.600(10)
_cell_formula_units_Z            2
_cell_length_a                   9.715(2)
_cell_length_b                   10.256(2)
_cell_length_c                   18.122(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1580.1(5)
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5347
_diffrn_reflns_theta_max         24.06
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.590
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       needles
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.867
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.958
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.959
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_obs          0.0507
_refine_ls_shift/esd_max         0.133
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1339
_refine_ls_wR_factor_obs         0.1253
_reflns_number_observed          3730
_reflns_number_total             4997
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            D802334sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+0.0000P] 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^)+(0.0881P)^2^+0.0000P] 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      P-1
_cod_database_code               7028003