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_7009122
_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         'C7 H15 Mo N3 S3'
_chemical_formula_structural     '[Mo(NNMe){N(CH2CH2S)3}]'
_chemical_formula_sum            'C7 H15 Mo N3 S3'
_chemical_formula_weight         333.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2a'
_symmetry_space_group_name_H-M   'P m c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4093(7)
_cell_length_b                   10.5438(10)
_cell_length_c                   14.0272(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     1243.74(19)
_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  0.009
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1604
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       'rectangular prisms'
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.126
_refine_ls_goodness_of_fit_obs   1.133
_refine_ls_hydrogen_treatment    'riding in idealised positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_restrained_S_obs      1.133
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_obs          0.0182
_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^)+(0.0152P)^2^+0.2556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0497
_refine_ls_wR_factor_obs         0.0475
_reflns_number_observed          1064
_reflns_number_total             1168
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908777j.txt
_cod_data_source_block           ray18
_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^)+(0.0152P)^2^+0.2556P] 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^)+(0.0152P)^2^+0.2556P] 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        1243.7(2)
_cod_original_sg_symbol_H-M      'Pmcn (equiv. to no. 62)             '
_cod_database_code               7009122