Molybdenum and tungsten complexes of the N(CH2CH2S)33− (NS3) ligand with oxide, sulfide, diazenide, hydrazide and nitrosyl co-ligands
Davies, Sian C.; Hughes, David L.; Richards, Raymond L.; Sanders, J. Roger; Journal of the Chemical Society, Dalton Transactions  (2000) 719–; doi:10.1039/a908777j

data_7009123
_publ_section_title
;
 Molybdenum and tungsten complexes of the N(CH2CH2S)33&#x2212; (NS3)
 ligand with oxide, sulfide, diazenide, hydrazide and nitrosyl
 co-ligands
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              719
_journal_paper_doi               10.1039/a908777j
_journal_year                    2000
_chemical_formula_moiety         'C12 H17 Mo N2 S3'
_chemical_formula_structural     '[Mo{N(CH2CH2S)3)}(NNPh)]'
_chemical_formula_sum            'C12 H17 Mo N3 S3'
_chemical_formula_weight         395.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'automated Patterson'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.000(9)
_cell_angle_beta                 90.000(8)
_cell_angle_gamma                90.000(8)
_cell_formula_units_Z            8
_cell_length_a                   15.1833(14)
_cell_length_b                   12.2873(14)
_cell_length_c                   16.861(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     3145.6(6)
_computing_cell_refinement       'CAD4/EXPRESS (Enraf-Nonius, 1992) '
_computing_data_collection       'CAD4/EXPRESS (Enraf-Nonius, 1992)  '
_computing_data_reduction        'CAD4 (Hursthouse, 1976)  '
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'scintillation counter; \w/\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3168
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        4.0
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.222
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            'Very dark red'
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       'diamond prisms'
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.994
_refine_ls_goodness_of_fit_obs   1.142
_refine_ls_hydrogen_treatment
;
 Coordinates were of idealised positions and set to ride on the parent carbon 
 atoms.  They were not included in the disordered phenyl ring with site
 occupancy of 0.2.  Isotropic thermal parameters were set to be 1.2 x Ueq
 of the parent carbons.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_restrained_S_obs      1.142
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_obs          0.0383
_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^)+(0.0418P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1137
_refine_ls_wR_factor_obs         0.0852
_reflns_number_observed          1266
_reflns_number_total             2759
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908777j.txt
_cod_data_source_block           ray20
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0418P)^2^] 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^)+(0.0418P)^2^]
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 c a b  (equiv. to no. 61)        '
_cod_database_code               7009123