#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/86/2008689.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2008689
loop_
_publ_author_name
'Ralf Hauptmann'
'Jörg Lackmann'
'Changneng Chen'
'Gerald Henkel'
_publ_section_title
;Di-μ-aqua-bis[(trimethanol-O)sodium]
 anti-bis(μ-2-propanethiolato-S:S)bis[bis(2-propanethiolato-S)iron(II)]
 and bis(benzyltrimethylammonium)
 anti-bis(μ-2-propaneselenolato-Se:Se)bis[bis(2-propaneselenolato-Se)iron(II)]
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1084
_journal_page_last               1087
_journal_paper_doi               10.1107/S0108270199003704
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac
'[Na2 (H2 O)2 (CH3 OH)6 ] ,[Fe2 (C3 H7 S)6 ]2'
_chemical_formula_moiety         'C24 H70 Fe2 Na2 O8 S6'
_chemical_formula_sum            'C24 H70 Fe2 Na2 O8 S6'
_chemical_formula_weight         836.84
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source
'International Tables for Crystallography (Vol. C)'
_cell_angle_alpha                113.89(4)
_cell_angle_beta                 112.11(4)
_cell_angle_gamma                95.83(4)
_cell_formula_units_Z            1
_cell_length_a                   10.516(7)
_cell_length_b                   11.484(6)
_cell_length_c                   11.705(7)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    150
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     1142.3(14)
_computing_cell_refinement       P3
_computing_data_collection       'P3 (Siemens, 1990a)'
_computing_data_reduction        'XDISK (Siemens, 1990b)'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measurement_device_type  'Siemens P4RA'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8099
_diffrn_reflns_theta_max         27.00
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 99
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(SHELXTL-Plus; Sheldrick, 1990)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columns
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.426
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         4982
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/esd_max         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0580P)²+0.6249P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1201
_reflns_number_gt                3914
_reflns_number_total             4982
_reflns_threshold_expression     F>4σ(F)
_cod_data_source_file            ka1304.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.6249P] 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^)+(0.0580P)^2^+0.6249P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2008689
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Fe -0.01390(4) 0.09705(4) 0.44363(4) 0.03080(13) Uani d . 1 . Fe
S1 -0.22615(8) 0.13738(8) 0.34201(8) 0.0381(2) Uani d . 1 . S
S2 0.18929(8) 0.21233(8) 0.45969(8) 0.0365(2) Uani d . 1 . S
S3 -0.04451(7) -0.13462(7) 0.32481(7) 0.0325(2) Uani d . 1 . S
C1 -0.1955(6) 0.3186(4) 0.4318(5) 0.085(2) Uani d . 1 . C
H1 -0.1018(6) 0.3478(4) 0.4406(5) 0.225(17) Uiso d R 1 . H
C2 -0.2715(8) 0.3684(5) 0.3413(6) 0.130(3) Uani d . 1 . C
H2A -0.2509(8) 0.4633(5) 0.3935(6) 0.225(17) Uiso d R 1 . H
H2B -0.2441(8) 0.3477(5) 0.2674(6) 0.225(17) Uiso d R 1 . H
H2C -0.3726(8) 0.3261(5) 0.3012(6) 0.225(17) Uiso d R 1 . H
C3 -0.1608(11) 0.3774(6) 0.5727(6) 0.162(4) Uani d . 1 . C
H3A -0.1464(11) 0.4717(6) 0.6096(6) 0.225(17) Uiso d R 1 . H
H3B -0.2382(11) 0.3386(6) 0.5831(6) 0.225(17) Uiso d R 1 . H
H3C -0.0743(11) 0.3619(6) 0.6232(6) 0.225(17) Uiso d R 1 . H
C4 0.1780(5) 0.1603(5) 0.2844(4) 0.0662(11) Uani d . 1 . C
H4 0.1760(5) 0.0684(5) 0.2461(4) 0.149(10) Uiso d R 1 . H
C5 0.0493(7) 0.1652(9) 0.1871(6) 0.142(3) Uani d . 1 . C
H5A 0.0481(7) 0.1363(9) 0.0974(6) 0.149(10) Uiso d R 1 . H
H5B -0.0331(7) 0.1088(9) 0.1763(6) 0.149(10) Uiso d R 1 . H
H5C 0.0465(7) 0.2558(9) 0.2241(6) 0.149(10) Uiso d R 1 . H
C6 0.3146(6) 0.2391(6) 0.3019(6) 0.097(2) Uani d . 1 . C
H6A 0.3111(6) 0.2133(6) 0.2116(6) 0.149(10) Uiso d R 1 . H
H6B 0.3239(6) 0.3325(6) 0.3474(6) 0.149(10) Uiso d R 1 . H
H6C 0.3957(6) 0.2219(6) 0.3587(6) 0.149(10) Uiso d R 1 . H
C7 -0.2374(3) -0.2281(3) 0.2062(3) 0.0380(7) Uani d . 1 . C
H7 -0.2920(3) -0.1925(3) 0.2546(3) 0.056(4) Uiso d R 1 . H
C8 -0.2852(4) -0.2098(4) 0.0768(3) 0.0541(9) Uani d . 1 . C
H8A -0.3854(4) -0.2573(4) 0.0148(3) 0.056(4) Uiso d R 1 . H
H8B -0.2295(4) -0.2437(4) 0.0292(3) 0.056(4) Uiso d R 1 . H
H8C -0.2698(4) -0.1165(4) 0.1047(3) 0.056(4) Uiso d R 1 . H
C9 -0.2607(4) -0.3734(3) 0.1692(4) 0.0537(9) Uani d . 1 . C
H9A -0.3606(4) -0.4231(3) 0.1084(4) 0.056(4) Uiso d R 1 . H
H9B -0.2297(4) -0.3804(3) 0.2539(4) 0.056(4) Uiso d R 1 . H
H9C -0.2049(4) -0.4089(3) 0.1224(4) 0.056(4) Uiso d R 1 . H
Na 0.59508(13) 0.12984(13) 0.67757(13) 0.0410(3) Uani d . 1 . Na
O1 0.3498(2) -0.0055(2) 0.5037(2) 0.0386(5) Uani d . 1 . O
H13A 0.2963(2) 0.0410(2) 0.4829(2) 0.090(7) Uiso d R 1 . H
H13B 0.3121(2) -0.0539(2) 0.5285(2) 0.090(7) Uiso d R 1 . H
O2 0.5220(2) 0.3104(2) 0.6772(3) 0.0562(7) Uani d . 1 . O
H14 0.4339(2) 0.2749(2) 0.6223(3) 0.090(7) Uiso d R 1 . H
O3 0.8391(3) 0.2278(3) 0.8246(3) 0.0802(10) Uani d . 1 . O
H15 0.8892(3) 0.1842(3) 0.7778(3) 0.090(7) Uiso d R 1 . H
O4 0.5510(3) 0.0547(3) 0.8154(3) 0.0653(8) Uani d . 1 . O
H16 0.4729(3) 0.0015(3) 0.7956(3) 0.090(7) Uiso d R 1 . H
C10 0.5816(5) 0.4494(4) 0.7377(5) 0.0755(13) Uani d . 1 . C
H10A 0.5085(5) 0.4893(4) 0.7078(5) 0.22(2) Uiso d R 1 . H
H10B 0.6258(5) 0.4880(4) 0.8383(5) 0.22(2) Uiso d R 1 . H
H10D 0.6531(5) 0.4654(4) 0.7092(5) 0.22(2) Uiso d R 1 . H
C11 0.9196(6) 0.3277(6) 0.9542(6) 0.112(2) Uani d . 1 . C
H11A 1.0194(6) 0.3378(6) 0.9781(6) 0.29(3) Uiso d R 1 . H
H11D 0.8991(6) 0.4086(6) 0.9588(6) 0.29(3) Uiso d R 1 . H
H11B 0.8986(6) 0.3092(6) 1.0192(6) 0.29(3) Uiso d R 1 . H
C12 0.6348(5) 0.0756(6) 0.9534(5) 0.086(2) Uani d . 1 . C
H12D 0.5797(5) 0.0252(6) 0.9766(5) 0.20(2) Uiso d R 1 . H
H12A 0.7200(5) 0.0492(6) 0.9605(5) 0.20(2) Uiso d R 1 . H
H12B 0.6614(5) 0.1690(6) 1.0174(5) 0.20(2) Uiso d R 1 . H
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 Fe S2 . . 117.85(6) yes
S1 Fe S3 . . 109.12(7) yes
S2 Fe S3 . . 108.89(6) yes
S1 Fe S3 . 2_556 112.34(5) yes
S2 Fe S3 . 2_556 105.86(7) yes
S3 Fe S3 . 2_556 101.49(6) yes
C1 S1 Fe . . 107.7(2) yes
C4 S2 Fe . . 111.06(15) yes
C7 S3 Fe . . 110.37(12) yes
C7 S3 Fe . 2_556 109.98(11) yes
Fe S3 Fe . 2_556 78.51(6) yes
C3 C1 C2 . . 122.9(5) no
C3 C1 S1 . . 116.6(4) no
C2 C1 S1 . . 113.9(4) no
C5 C4 C6 . . 114.0(5) no
C5 C4 S2 . . 113.7(4) no
C6 C4 S2 . . 108.6(3) no
C9 C7 C8 . . 112.1(3) no
C9 C7 S3 . . 109.5(2) no
C8 C7 S3 . . 109.3(2) no
O4 Na O2 . . 116.27(12) yes
O4 Na O3 . . 95.45(13) yes
O2 Na O3 . . 101.38(13) yes
O4 Na O1 . 2_656 124.26(12) yes
O2 Na O1 . 2_656 117.35(11) yes
O3 Na O1 . 2_656 88.19(11) yes
O4 Na O1 . . 85.11(10) yes
O2 Na O1 . . 86.84(10) yes
O3 Na O1 . . 170.44(11) yes
O1 Na O1 2_656 . 83.66(10) yes
O4 Na Na . 2_656 108.27(11) no
O2 Na Na . 2_656 105.41(10) no
O3 Na Na . 2_656 130.64(10) no
O1 Na Na 2_656 2_656 42.65(7) no
O1 Na Na . 2_656 41.01(7) no
Na O1 Na 2_656 . 96.34(10) no
C10 O2 Na . . 139.0(2) no
C11 O3 Na . . 135.2(3) no
C12 O4 Na . . 133.8(3) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe S1 . 2.295(2) yes
Fe S2 . 2.297(2) yes
Fe S3 . 2.368(2) yes
Fe S3 2_556 2.378(2) yes
S1 C1 . 1.837(4) no
S2 C4 . 1.841(4) no
S3 C7 . 1.851(3) no
S3 Fe 2_556 2.378(2) no
C1 C3 . 1.380(7) no
C1 C2 . 1.426(6) no
C4 C5 . 1.428(7) no
C4 C6 . 1.513(6) no
C7 C9 . 1.512(5) no
C7 C8 . 1.516(5) no
Na O4 . 2.274(3) yes
Na O2 . 2.284(3) yes
Na O3 . 2.310(4) yes
Na O1 2_656 2.349(3) yes
Na O1 . 2.426(3) yes
Na Na 2_656 3.558(4) yes
O1 Na 2_656 2.349(3) no
O2 C10 . 1.411(5) no
O3 C11 . 1.326(6) no
O4 C12 . 1.420(5) no
