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_7011090
_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         'C16 H36 N, C13 H24 N3 S6 V2, 2(C2 H3 N)'
_chemical_formula_structural     (NBu4)[{N(CH2CH2S)3}VCNV{N(CH2CH2S)3}].2MeCN
_chemical_formula_sum            'C33 H66 N6 S6 V2'
_chemical_formula_weight         841.16
_chemical_name_common            'Complex 4'
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 100.518(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.6163(14)
_cell_length_b                   17.384(2)
_cell_length_c                   11.3268(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     2248.9(5)
_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 CAD 4-circle diffractometer'
_diffrn_measurement_method       bisecting
_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  0.01840
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2819
_diffrn_reflns_theta_max         20
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        6
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.112
_exptl_absorpt_correction_T_min  0.094
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            'Dark orange-brown'
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       'subhedral plate'
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.082
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment
;
Coordinates were set to ride on the parent carbon atoms, those of the
methyl hydrogens in rotating groups and those of the ethyl hydrogens in 
idealised positions.  Thermal parameters of the ethyl 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.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         2167
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.090
_refine_ls_restrained_S_obs      1.116
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_obs          0.0371
_refine_ls_shift/esd_max         0.425
_refine_ls_shift/esd_mean        0.089
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.4733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1034
_refine_ls_wR_factor_obs         0.0898
_reflns_number_observed          1677
_reflns_number_total             2167
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b107399k.txt
_cod_data_source_block           roger14x
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.4733P] 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^)+(0.0542P)^2^+0.4733P] 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        2248.9(4)
_cod_original_sg_symbol_H-M      'P 21  '
_cod_database_code               7011090