Diaqua(1,4,7,10,13-pentaoxacyclopentadecane)iron(II) bis(μ-<i>cis</i>-1,2-dicyano-1,2-ethylenedithiolato)bis[(<i>cis</i>-1,2-dicyano-1,2-ethylenedithiolato)ferrate(III)] 1,4,7,10,13-pentaoxacyclopentadecane disolvate
Yamaguchi, Toshiki; Masaoka, Shigeyuki; Sakai, Ken; Acta Crystallographica Section E 64 (2008) m1557–m1558; doi:10.1107/S1600536808036805

data_2220271
_publ_section_title
;Diaqua(1,4,7,10,13-pentaoxacyclopentadecane)iron(II)
 bis(\m-<i>cis</i>-1,2-dicyano-1,2-ethylenedithiolato)bis[(<i>cis</i>-1,2-dicyano-1,2-ethylenedithiolato)ferrate(III)]
 1,4,7,10,13-pentaoxacyclopentadecane disolvate
;
_journal_coeditor_code           LH2727
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1557
_journal_page_last               m1558
_journal_paper_doi               10.1107/S1600536808036805
_journal_volume                  64
_journal_year                    2008
_chemical_formula_analytical     'C46 H64 Fe3 N8 O17 S8'
_chemical_formula_iupac
'[Fe (C10 H20 O5) (H2 O)2] [Fe2 (C4 N2 S2)4], 2C10 H20 O5'
_chemical_formula_moiety
'C10 H24 Fe O7 2+, C16 Fe2 N8 2- S8, 2(C10 H20 O5)'
_chemical_formula_structural     'C46 H64 Fe3 N8 O17 S8'
_chemical_formula_sum            'C46 H64 Fe3 N8 O17 S8'
_chemical_formula_weight         1425.08
_chemical_name_systematic
;
Diaqua(1,4,7,10,13-pentaoxacyclopentadecane)iron(II)
bis(\m-<i>cis</i>-1,2-dicyano-1,2-ethylenedithiolato)bis[(<i>cis</i>-
1,2-dicyano-1,2-ethylenedithiolato)ferrate(III)]
1,4,7,10,13-pentaoxacyclopentadecane disolvate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.600(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.376(4)
_cell_length_b                   15.739(4)
_cell_length_c                   30.069(8)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.39
_cell_volume                     6328(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'KENX (Sakai, 2004)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), TEXSAN (Molecular Structure Corporation,
2001),
KENX (Sakai, 2004) and ORTEPII (Johnson, 1976)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode with a mirror focusing unit'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            68765
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.339
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         13837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+3.2078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                10591
_reflns_number_total             13837
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2727.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2220271
_cod_database_fobs_code          2220271