#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/87/7018707.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7018707
loop_
_publ_author_name
'Abrahams, Brendan F.'
'Abrahams, Carmel T.'
'Haywood, Marissa G.'
'Hudson, Timothy A.'
'Moubaraki, Boujemaa'
'Murray, Keith S.'
'Robson, Richard'
_publ_section_title
;
 3d-Metal derivatives of the [Cu(I)(SO(3))(4)](7-) ion: structure and
 magnetism.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4091
_journal_page_last               4099
_journal_paper_doi               10.1039/c2dt12337a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety
'(Cu S4 O12 7-)2, (Fe3 O4 H6 7+), (Fe H12 O6 2+)2, (Na3 H12 O6 3+), (H2 O)'
_chemical_formula_sum            'Cu2 Fe5 H44 Na3 O47 S8'
_chemical_formula_weight         1528.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   9.0550(3)
_cell_length_b                   9.0550(3)
_cell_length_c                   29.545(2)
_cell_measurement_reflns_used    6435
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     2097.93(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            12889
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        1.000
_exptl_absorpt_coefficient_mu    3.238
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.722523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SHELDRICK G. M. SADABS
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1534
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.781
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.388
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1643
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.385
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0152P)²+25.4812P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1336
_reflns_number_gt                1600
_reflns_number_total             1643
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12337a.txt
_cod_data_source_block           fe32871m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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_cell_volume        2097.9(2)
_cod_original_sg_symbol_H-M      P63/m
_cod_original_formula_sum        'H44 Cu2 Fe5 Na3 O47 S8'
_cod_database_code               7018707
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.6667 0.3333 0.14043(4) 0.0130(3) Uani 1 3 d S
Fe1 Fe 0.6667 0.3333 -0.09023(5) 0.0077(3) Uani 1 3 d S
Fe3 Fe 0.47847(16) 0.38677(15) 0.2500 0.0125(3) Uani 1 2 d S
S4 S 0.6667 0.3333 0.06429(8) 0.0101(5) Uani 1 3 d S
S5 S 0.40353(18) 0.13142(18) 0.16974(5) 0.0115(3) Uani 1 1 d .
O1 O 0.2618(6) 0.0225(6) 0.13882(15) 0.0165(9) Uani 1 1 d .
O2 O 0.3340(5) 0.2123(6) 0.20237(15) 0.0155(9) Uani 1 1 d .
O3 O 0.8336(5) 0.4661(6) 0.04447(15) 0.0161(9) Uani 1 1 d .
O4 O 0.1794(6) 0.1990(6) 0.05299(16) 0.0164(9) Uani 1 1 d D
O6 O 0.4310(6) 0.0059(6) 0.19943(15) 0.0153(9) Uani 1 1 d .
O7 O 0.8605(6) 0.5135(6) -0.04702(15) 0.0153(9) Uani 1 1 d D
O9 O 0.6667 0.3333 0.2500 0.017(2) Uani 1 6 d S
O10 O 0.2684(9) 0.4376(10) 0.2500 0.0213(14) Uani 1 2 d SD
O11 O 0.0000 0.0000 0.2500 0.046(4) Uani 1 6 d S
O12 O 0.6831(6) 0.5297(6) -0.13072(17) 0.0175(9) Uani 1 1 d D
Na2 Na 0.0000 0.0000 0.10797(15) 0.0139(8) Uani 1 3 d S
Na6 Na 0.0000 0.0000 0.0000 0.0087(11) Uani 1 6 d S
H41 H 0.171(11) 0.288(7) 0.049(3) 0.033(17) Uiso 1 1 d D
H42 H 0.287(3) 0.247(11) 0.058(3) 0.033(17) Uiso 1 1 d D
H71 H 0.961(4) 0.530(8) -0.050(2) 0.003(11) Uiso 1 1 d D
H72 H 0.848(8) 0.496(8) -0.0182(8) 0.003(11) Uiso 1 1 d D
H101 H 0.230(12) 0.443(13) 0.2239(16) 0.04(3) Uiso 1 1 d D
H121 H 0.785(5) 0.603(10) -0.139(3) 0.05(2) Uiso 1 1 d D
H122 H 0.637(12) 0.535(13) -0.1555(19) 0.05(2) Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S4 Cu1 S5 111.85(5) . 2_655
S4 Cu1 S5 111.85(5) . .
S5 Cu1 S5 106.99(5) 2_655 .
S4 Cu1 S5 111.85(5) . 3_665
S5 Cu1 S5 106.99(5) 2_655 3_665
S5 Cu1 S5 106.99(5) . 3_665
O9 Fe3 O2 96.17(13) . .
O9 Fe3 O2 96.17(13) . 10_556
O2 Fe3 O2 87.8(3) . 10_556
O9 Fe3 O6 97.06(13) . 3_665
O2 Fe3 O6 88.32(17) . 3_665
O2 Fe3 O6 166.53(19) 10_556 3_665
O9 Fe3 O6 97.06(13) . 12_666
O2 Fe3 O6 166.53(18) . 12_666
O2 Fe3 O6 88.32(17) 10_556 12_666
O6 Fe3 O6 92.5(2) 3_665 12_666
O9 Fe3 O10 178.4(2) . .
O2 Fe3 O10 82.71(19) . .
O2 Fe3 O10 82.71(19) 10_556 .
O6 Fe3 O10 84.01(19) 3_665 .
O6 Fe3 O10 84.01(19) 12_666 .
O3 S4 O3 105.8(2) 3_665 .
O3 S4 O3 105.8(2) 3_665 2_655
O3 S4 O3 105.8(2) . 2_655
O3 S4 Cu1 112.94(19) 3_665 .
O3 S4 Cu1 112.94(19) . .
O3 S4 Cu1 112.94(19) 2_655 .
O1 S5 O2 106.4(3) . .
O1 S5 O6 105.3(3) . .
O2 S5 O6 104.5(2) . .
O1 S5 Cu1 120.0(2) . .
O2 S5 Cu1 111.38(18) . .
O6 S5 Cu1 108.04(18) . .
S5 O2 Fe3 123.5(3) . .
S5 O6 Fe3 121.6(3) . 2_655
S5 O1 Na2 140.0(3) . .
O12 Fe1 O12 90.38(19) 3_665 2_655
O12 Fe1 O12 90.38(19) 3_665 .
O12 Fe1 O12 90.38(19) 2_655 .
O12 Fe1 O7 91.40(18) 3_665 .
O12 Fe1 O7 177.95(19) 2_655 .
O12 Fe1 O7 90.60(17) . .
O12 Fe1 O7 90.60(17) 3_665 3_665
O12 Fe1 O7 91.40(18) 2_655 3_665
O12 Fe1 O7 177.95(19) . 3_665
O7 Fe1 O7 87.58(18) . 3_665
O12 Fe1 O7 177.95(19) 3_665 2_655
O12 Fe1 O7 90.60(17) 2_655 2_655
O12 Fe1 O7 91.40(18) . 2_655
O7 Fe1 O7 87.58(18) . 2_655
O7 Fe1 O7 87.58(18) 3_665 2_655
O4 Na6 O4 79.65(18) 7 9
O4 Na6 O4 79.65(18) 7 8
O4 Na6 O4 79.65(18) 9 8
O4 Na6 O4 180.0(3) 7 .
O4 Na6 O4 100.35(18) 9 .
O4 Na6 O4 100.35(18) 8 .
O4 Na6 O4 100.35(18) 7 2
O4 Na6 O4 100.35(18) 9 2
O4 Na6 O4 180.00(18) 8 2
O4 Na6 O4 79.65(18) . 2
O4 Na6 O4 100.35(18) 7 3
O4 Na6 O4 180.00(18) 9 3
O4 Na6 O4 100.35(18) 8 3
O4 Na6 O4 79.65(18) . 3
O4 Na6 O4 79.65(18) 2 3
O4 Na6 Na2 47.69(12) 7 7
O4 Na6 Na2 47.69(12) 9 7
O4 Na6 Na2 47.69(12) 8 7
O4 Na6 Na2 132.31(12) . 7
O4 Na6 Na2 132.31(12) 2 7
O4 Na6 Na2 132.31(12) 3 7
O4 Na6 Na2 132.31(12) 7 .
O4 Na6 Na2 132.31(12) 9 .
O4 Na6 Na2 132.31(12) 8 .
O4 Na6 Na2 47.69(12) . .
O4 Na6 Na2 47.69(12) 2 .
O4 Na6 Na2 47.69(12) 3 .
Na2 Na6 Na2 180.0 7 .
Na6 O4 Na2 85.68(17) . .
O4 Na2 O4 78.0(2) 2 3
O4 Na2 O4 78.0(2) 2 .
O4 Na2 O4 78.0(2) 3 .
O4 Na2 O1 158.5(2) 2 .
O4 Na2 O1 84.90(15) 3 .
O4 Na2 O1 85.68(16) . .
O4 Na2 O1 84.90(15) 2 3
O4 Na2 O1 85.68(16) 3 3
O4 Na2 O1 158.5(2) . 3
O1 Na2 O1 107.01(15) . 3
O4 Na2 O1 85.68(15) 2 2
O4 Na2 O1 158.5(2) 3 2
O4 Na2 O1 84.90(15) . 2
O1 Na2 O1 107.01(15) . 2
O1 Na2 O1 107.01(15) 3 2
O4 Na2 Na6 46.63(13) 2 .
O4 Na2 Na6 46.64(13) 3 .
O4 Na2 Na6 46.63(13) . .
O1 Na2 Na6 111.83(14) . .
O1 Na2 Na6 111.83(14) 3 .
O1 Na2 Na6 111.83(14) 2 .
Fe3 O9 Fe3 120.0 2_655 3_665
Fe3 O9 Fe3 120.000(1) 2_655 .
Fe3 O9 Fe3 120.0 3_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 S4 2.250(3) .
Cu1 S5 2.3267(15) 2_655
Cu1 S5 2.3267(15) .
Cu1 S5 2.3267(15) 3_665
Fe3 O9 1.9907(13) .
Fe3 O2 2.030(5) .
Fe3 O2 2.030(5) 10_556
Fe3 O6 2.068(4) 3_665
Fe3 O6 2.068(4) 12_666
Fe3 O10 2.169(7) .
S4 O3 1.502(4) 3_665
S4 O3 1.502(4) .
S4 O3 1.502(4) 2_655
S5 O1 1.480(4) .
S5 O2 1.524(4) .
S5 O6 1.551(4) .
O6 Fe3 2.068(4) 2_655
O1 Na2 2.451(5) .
Fe1 O12 2.086(5) 3_665
Fe1 O12 2.086(5) 2_655
Fe1 O12 2.086(5) .
Fe1 O7 2.123(5) .
Fe1 O7 2.123(5) 3_665
Fe1 O7 2.123(5) 2_655
Na6 O4 2.326(5) 7
Na6 O4 2.326(5) 9
Na6 O4 2.326(5) 8
Na6 O4 2.326(5) .
Na6 O4 2.326(5) 2
Na6 O4 2.326(5) 3
Na6 Na2 3.190(4) 7
Na6 Na2 3.190(4) .
O4 Na2 2.366(6) .
Na2 O4 2.366(6) 2
Na2 O4 2.366(6) 3
Na2 O1 2.451(5) 3
Na2 O1 2.451(5) 2
O9 Fe3 1.9907(13) 2_655
O9 Fe3 1.9907(13) 3_665
