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_7009121
_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 H24 Mo2 N2 S7, 0.3(H2 O)'
_chemical_formula_structural     '[(Mo{N(CH2CH2S)3})2(mu-S)].0.3H2O'
_chemical_formula_sum            'C12 H24.6 Mo2 N2 O0.3 S7'
_chemical_formula_weight         618.0
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_space_group_name_H-M   'R -3 :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                77.833(7)
_cell_angle_beta                 77.833(7)
_cell_angle_gamma                77.833(7)
_cell_formula_units_Z            1
_cell_length_a                   8.3292(5)
_cell_length_b                   8.3292(5)
_cell_length_c                   8.3292(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9.4
_cell_volume                     543.74(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  0.030
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3814
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.83
_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    1.887
_exptl_crystal_description       rhombs
_exptl_crystal_F_000             309
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.147
_refine_ls_goodness_of_fit_obs   1.187
_refine_ls_hydrogen_treatment    'riding, in idealised positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_restrained_S_obs      1.187
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_obs          0.0242
_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^)+(0.0272P)^2^+0.3071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0741
_refine_ls_wR_factor_obs         0.0723
_reflns_number_observed          573
_reflns_number_total             641
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908777j.txt
_cod_data_source_block           ray19
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
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^)+(0.0272P)^2^+0.3071P] 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^)+(0.0272P)^2^+0.3071P] 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        543.74(7)
_cod_original_sg_symbol_H-M      'R-3 (no. 148)'
_cod_database_code               7009121