Iron, cobalt and vanadium complexes of the N(CH2CH2S)33− ligand with chloride, azide, cyanide and carbonyl co-ligands
Davies, Sian C.; Durrant, Marcus C.; Hughes, David L.; Richards, Raymond L.; Sanders, J. Roger; Journal of the Chemical Society, Dalton Transactions  (2000) 4694–; doi:10.1039/b006591i

data_7010161
_publ_section_title
;
 Iron, cobalt and vanadium complexes of the N(CH2CH2S)33&#x2212; ligand
 with chloride, azide, cyanide and carbonyl co-ligands
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4694
_journal_paper_doi               10.1039/b006591i
_journal_year                    2000
_chemical_formula_moiety         'C8 H20 N, C6 H12 Fe N4 S3'
_chemical_formula_structural     (NEt4)[Fe(N3)(NS3)]
_chemical_formula_sum            'C14 H32 Fe N5 S3'
_chemical_formula_weight         422.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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            8
_cell_length_a                   15.905(2)
_cell_length_b                   14.2539(15)
_cell_length_c                   18.458(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     4184.6(10)
_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  0.011
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2732
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        5.7
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  0.033
_exptl_absorpt_correction_T_min  0.014
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            'dark reddish-brown'
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       rhombohedra
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.143
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         2534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_restrained_S_obs      1.143
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_obs          0.0473
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0613P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1275
_refine_ls_wR_factor_obs         0.1070
_reflns_number_observed          1620
_reflns_number_total             2534
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006591i.txt
_cod_data_source_block           roger40
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0613P)^2^] 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^)+(0.0613P)^2^]
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        4184.8(10)
_cod_original_sg_symbol_H-M      'C 2 2 21 (no. 20)'
_cod_database_code               7010161