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_7010160
_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 Cl Fe N S3'
_chemical_formula_structural     (NEt4)[Fe(Cl){N(CH2CH2S)3}]
_chemical_formula_sum            'C14 H32 Cl Fe N S3'
_chemical_formula_weight         415.9
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.002(7)
_cell_angle_beta                 89.993(8)
_cell_angle_gamma                89.992(8)
_cell_formula_units_Z            4
_cell_length_a                   8.7922(9)
_cell_length_b                   14.3189(11)
_cell_length_c                   15.9028(14)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     2002.1(3)
_computing_cell_refinement       'CAD4/EXPRESS (Enraf-Nonius)'
_computing_data_collection       'CAD4/EXPRESS (Enraf-Nonius)'
_computing_data_reduction        'CAD4, EMPABS, BAYES, SHELX-76'
_computing_molecular_graphics    'UNITEK, ORTEP, Windows DRAW'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       '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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2736
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        6.66
_diffrn_standards_interval_count 10000
_diffrn_standards_interval_time  300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.398
_exptl_absorpt_correction_T_min  0.331
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       'irregular hexagonal prisms'
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_hydrogen_treatment
;
 Hydrogen atoms were included in idealised positions and set to ride on the 
 coordinates of the parent carbon atoms.  The Uiso's of the hydrogens on the 
 anion were refined freely, whereas those on the disordered cations were set 
 to ride on those of the parent carbon atoms.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_restrained_S_obs      1.115
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_obs          0.0396
_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^)+(0.0500P)^2^+0.6970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1125
_refine_ls_wR_factor_obs         0.1008
_reflns_number_observed          1870
_reflns_number_total             2504
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006591i.txt
_cod_data_source_block           roger24
_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^)+(0.0500P)^2^+0.6970P] 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^)+(0.0500P)^2^+0.6970P] 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 b c m   (no. 57)'
_cod_database_code               7010160