Dinuclear iron and vanadium complexes of the N(CH2CH2S)33− ligand with bridging oxide, nitride or cyanide
Sian C. Davies; David L. Hughes; Raymond L. Richards; J. Roger Sanders; J. Chem. Soc., Dalton Trans.  (2002) 1442–1447; doi:10.1039/b107399k

data_7011091
_publ_section_title
;
 Dinuclear iron and vanadium complexes of the N(CH2CH2S)33&#x2212;
 ligand with bridging oxide, nitride or cyanide
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1442
_journal_page_last               1447
_journal_paper_doi               10.1039/b107399k
_journal_year                    2002
_chemical_formula_moiety         'C8 H20 N, C7 H12 Fe N2 S3'
_chemical_formula_structural     (NEt4)[Fe(CN)(N{CH2CH2S}3)]
_chemical_formula_sum            'C15 H32 Fe N3 S3'
_chemical_formula_weight         406.47
_chemical_name_common            'Complex 6'
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'isostructural with Co analogue'
_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                   8.9215(9)
_cell_length_b                   14.1773(14)
_cell_length_c                   15.7017(13)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     1986.0(3)
_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       '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           Mo-K\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2209
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        1.3
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.209
_exptl_absorpt_correction_T_min  0.174
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       needles
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment
; 
Hydrogen coordinates were of idealised positions and set to ride on the
parent carbon atoms.  All isotropic thermal displacement parameters were 
set to be 1.2 x Ueq of the parent atoms.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_obs          0.0460
_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^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1232
_refine_ls_wR_factor_obs         0.0994
_reflns_number_observed          1031
_reflns_number_total             1821
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b107399k.txt
_cod_data_source_block           roger49
_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^)+(0.0510P)^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^)+(0.0510P)^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_database_code               7011091