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_7028002
_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            'C22 H21 Mo N3 O2 S3'
_chemical_formula_weight         551.54
_chemical_name_common
;
cis-Dioxo-(S-benzyl-3-(2-mercapto-phenyl)-methylendithiocarbazate)
(4-methyl-pyridine)molybdenum(VI) 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.89(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.779(2)
_cell_length_b                   12.678(2)
_cell_length_c                   17.567(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2357.4(7)
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5446
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.846
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       needles
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.355
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.887
_refine_ls_goodness_of_fit_obs   1.007
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_restrained_S_obs      1.007
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_obs          0.0375
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0902
_refine_ls_wR_factor_obs         0.0839
_reflns_number_observed          3544
_reflns_number_total             5160
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            D802334sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0488P)^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^)+(0.0488P)^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      P2(1)/c
_cod_database_code               7028002