X-Ray crystallographic analysis of D,L-[Fe2{SCH2CH(CH2OH)S}(CO)6] reveals a hydrogen-bonded cyclic hexamer with ordered optical centres
Razavet, Mathieu; Cloirec, Alban Le; Davies, Sian C.; Hughes, David L.; Pickett, Christopher J.; Journal of the Chemical Society, Dalton Transactions  (2001) 3551–; doi:10.1039/b107595k

data_7011106
_publ_section_title
;
 X-Ray crystallographic analysis of D,L-[Fe2{SCH2CH(CH2OH)S}(CO)6]
 reveals a hydrogen-bonded cyclic hexamer with ordered optical centres
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3551
_journal_paper_doi               10.1039/b107595k
_journal_year                    2001
_chemical_formula_moiety         'C9 H6 Fe2 O7 S2'
_chemical_formula_structural     '[{Fe(CO)3}2{mu-SCH2CH(CH2OH)S}]'
_chemical_formula_sum            'C9 H6 Fe2 O7 S2'
_chemical_formula_weight         401.96
_chemical_name_common            mathieu1
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-F 1'
_space_group_name_H-M_alt        'F -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                97.249(9)
_cell_angle_beta                 102.212(8)
_cell_angle_gamma                94.503(9)
_cell_formula_units_Z            24
_cell_length_a                   18.834(2)
_cell_length_b                   26.405(3)
_cell_length_c                   18.300(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     8771.7(17)
_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  0.0093
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13149
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.29
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            'Dark orange'
_exptl_crystal_density_diffrn    1.83
_exptl_crystal_description       prisms
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment
;
Hydrogen coordinates were initially located in idealised postions except those
of the hydroxyl hydrogens, which were located from electron density maps; all
were subsequently refined freely.  All isotropic thermal parameters were 
refined freely.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         12750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_obs          0.0314
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0169P)^2^+8.7313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0790
_refine_ls_wR_factor_obs         0.0675
_reflns_number_observed          8642
_reflns_number_total             12750
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b107595k.txt
_cod_data_source_block           mathieu1
_cod_depositor_comments
;
 Updating space group information.

 2018-06-13,
 Antanas Vaitkus

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0169P)^2^+8.7313P] 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^)+(0.0169P)^2^+8.7313P] 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        8772.0(15)
_cod_database_code               7011106