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_7011088
_publ_section_title
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 Dinuclear iron and vanadium complexes of the N(CH2CH2S)33&#x2212;
 ligand with bridging oxide, nitride or cyanide
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_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         '2(C8 H20 N), C12 H24 Fe2 N2 O S6, C2 H3 N'
_chemical_formula_structural     (NEt4)2[(Fe{N(CH2CH2S)3})2(mu-O)]
_chemical_formula_sum            'C30 H67 Fe2 N5 O S6'
_chemical_formula_weight         817.95
_chemical_name_common            'Complex 1'
_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                 92.207(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9292(15)
_cell_length_b                   11.2912(10)
_cell_length_c                   22.060(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     4213.7(7)
_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  0.014
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8213
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        11.0
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            'Reddish brown'
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       'square and hexagonal prisms'
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.137
_refine_ls_hydrogen_treatment
;
Coordinates were of idealised positions and set to ride on the parent
carbon atoms.  Isotropic thermal parameters of the ethylene hydrogens 
were set to be 1.2 x Ueq of the parent carbon atoms and those of the 
methyl hydrogens were set to be 1.5 x Ueq of the parent atoms.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.137
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_obs          0.0417
_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^)+(0.0358P)^2^+1.1454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1095
_refine_ls_wR_factor_obs         0.0889
_reflns_number_observed          4389
_reflns_number_total             7390
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b107399k.txt
_cod_data_source_block           roger29
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+1.1454P] 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^)+(0.0358P)^2^+1.1454P] 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 21/c'
_cod_database_code               7011088