#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/58/2005845.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_2005845
loop_
_publ_author_name
'Longridge, J. J.'
'Rawson, J. M.'
'Davies, J. E.'
_publ_section_title
;
 A Mixed Cation Ternary Nitroprusside:
 [(CH₃)₄N][Na][Fe(CN)₅(NO)].2.5H₂O
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              15
_journal_page_last               17
_journal_paper_doi               10.1107/S0108270196011468
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac
'[(CH3)4 N] +, Na +, [Fe(CN)5(NO)] 2-, 2.5(H2O)'
_chemical_formula_structural     '(C4 H12 N) Na [Fe (C N)5 (N O)] , 2.5H2 O '
_chemical_formula_sum            'C9 H17 Fe N7 Na O3.5'
_chemical_formula_weight         358.14
_chemical_name_common
;
tetramethylammonium sodium nitroprusside 2.5-hydrate
;
_chemical_name_systematic
;
tetramethylammonium sodium nitrosylpentacyanoferrate (II) 2.5-hydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.57(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.454(4)
_cell_length_b                   9.107(2)
_cell_length_c                   17.364(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40
_cell_measurement_theta_min      30
_cell_volume                     3386.0(11)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
1988)
;
_computing_data_reduction
'TEXSAN PROCESS (Molecular Structure Corporation, 1985)'
_computing_molecular_graphics    'XP (Siemens, 1994)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC-7R diffractometer'
_diffrn_measurement_method       'ω-2θ 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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2837
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.086
_refine_ls_goodness_of_fit_obs   1.140
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2490
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.093
_refine_ls_restrained_S_obs      1.141
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_obs          0.0477
_refine_ls_shift/esd_max         0.307
_refine_ls_shift/esd_mean        0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.049P)²+8.61P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1259
_refine_ls_wR_factor_obs         0.1155
_reflns_number_observed          1961
_reflns_number_total             2494
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1089.cif
_cod_data_source_block           jr9601
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.049P)^2^+8.61P] 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^)+(0.049P)^2^+8.61P] 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      C2/c
_cod_original_formula_sum        'C9 H17 Fe N7 Na O3.50'
_cod_database_code               2005845
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_occupancy
_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_disorder_group
_atom_site_type_symbol
Fe1 1 0.08062(3) 0.02356(6) 0.12291(3) 0.0346(2) Uani d . . Fe
N 1 0.0049(2) 0.0563(4) 0.1251(2) 0.0437(9) Uani d . . N
C1 1 0.0848(2) -0.1026(5) 0.2128(3) 0.0457(11) Uani d . . C
N3 1 0.2225(2) -0.0219(6) 0.1221(3) 0.0718(13) Uani d . . N
C2 1 0.0908(2) 0.1425(5) 0.0314(3) 0.0434(11) Uani d . . C
C3 1 0.1697(2) -0.0054(5) 0.1224(2) 0.0454(11) Uani d . . C
O 1 -0.0461(2) 0.0849(5) 0.1282(2) 0.0742(11) Uani d . . O
N2 1 0.0964(2) 0.2106(5) -0.0223(2) 0.0660(12) Uani d . . N
C4 1 0.1023(2) 0.1883(5) 0.1892(3) 0.0460(11) Uani d . . C
C5 1 0.0739(2) -0.1511(6) 0.0594(3) 0.0549(13) Uani d . . C
N5 1 0.0707(3) -0.2559(6) 0.0231(3) 0.092(2) Uani d . . N
N1 1 0.0867(2) -0.1772(5) 0.2657(2) 0.0686(13) Uani d . . N
N4 1 0.1141(2) 0.2838(5) 0.2301(3) 0.0758(14) Uani d . . N
N12 1 0.2434(2) 0.5140(4) 0.1166(2) 0.0471(9) Uani d D . N
C12A 0.368(10) 0.2954(10) 0.602(3) 0.0829(14) 0.098(2) Uani d PD 1 C
H12A 0.368(10) 0.2893(43) 0.7049(31) 0.0928(83) 0.146 Uiso calc PR 1 H
H12B 0.368(10) 0.2948(49) 0.5861(144) 0.0282(20) 0.146 Uiso calc PR 1 H
H12C 0.368(10) 0.3350(12) 0.5718(126) 0.1064(69) 0.146 Uiso calc PR 1 H
C13A 0.368(10) 0.2386(10) 0.547(2) 0.1973(8) 0.098(2) Uani d PD 1 C
H13A 0.368(10) 0.2317(70) 0.6498(33) 0.2036(12) 0.146 Uiso calc PR 1 H
H13B 0.368(10) 0.2767(28) 0.5187(153) 0.2256(15) 0.146 Uiso calc PR 1 H
H13C 0.368(10) 0.2044(45) 0.4927(126) 0.2164(23) 0.146 Uiso calc PR 1 H
C14A 0.368(10) 0.1850(8) 0.554(2) 0.0701(11) 0.098(2) Uani d PD 1 C
H14A 0.368(10) 0.1556(27) 0.4748(70) 0.0713(70) 0.146 Uiso calc PR 1 H
H14B 0.368(10) 0.1946(13) 0.5728(158) 0.0177(23) 0.146 Uiso calc PR 1 H
H14C 0.368(10) 0.1672(38) 0.6407(97) 0.0914(53) 0.146 Uiso calc PR 1 H
C15A 0.368(10) 0.2579(9) 0.3555(17) 0.1003(13) 0.098(2) Uani d PD 1 C
H15A 0.368(10) 0.2984(28) 0.3313(45) 0.1234(70) 0.146 Uiso calc PR 1 H
H15B 0.368(10) 0.2575(66) 0.3405(38) 0.0455(13) 0.146 Uiso calc PR 1 H
H15C 0.368(10) 0.2270(37) 0.2938(19) 0.1215(72) 0.146 Uiso calc PR 1 H
C12B 0.632(10) 0.2962(6) 0.6092(17) 0.0992(8) 0.098(2) Uani d PD 2 C
H12D 0.632(10) 0.2807(7) 0.6972(49) 0.0743(50) 0.146 Uiso calc PR 2 H
H12E 0.632(10) 0.3228(24) 0.5582(41) 0.0656(45) 0.146 Uiso calc PR 2 H
H12F 0.632(10) 0.3197(27) 0.6342(87) 0.1463(10) 0.146 Uiso calc PR 2 H
C13B 0.632(10) 0.2050(6) 0.5875(13) 0.1771(7) 0.098(2) Uani d PD 2 C
H13D 0.632(10) 0.1729(26) 0.5215(39) 0.1918(37) 0.146 Uiso calc PR 2 H
H13E 0.632(10) 0.1862(34) 0.6755(53) 0.1559(18) 0.146 Uiso calc PR 2 H
H13F 0.632(10) 0.2318(10) 0.6118(88) 0.2216(22) 0.146 Uiso calc PR 2 H
C14B 0.632(10) 0.2003(5) 0.4885(14) 0.0488(6) 0.098(2) Uani d PD 2 C
H14D 0.632(10) 0.2213(13) 0.4341(82) 0.0108(21) 0.146 Uiso calc PR 2 H
H14E 0.632(10) 0.1866(31) 0.5810(14) 0.0274(29) 0.146 Uiso calc PR 2 H
H14F 0.632(10) 0.1649(20) 0.4336(80) 0.0639(11) 0.146 Uiso calc PR 2 H
C15B 0.632(10) 0.2677(5) 0.3741(12) 0.1496(8) 0.098(2) Uani d PD 2 C
H15D 0.632(10) 0.2929(32) 0.3265(46) 0.1133(21) 0.146 Uiso calc PR 2 H
H15E 0.632(10) 0.2334(5) 0.3114(38) 0.1606(45) 0.146 Uiso calc PR 2 H
H15F 0.632(10) 0.2925(33) 0.3935(14) 0.1964(27) 0.146 Uiso calc PR 2 H
Na1 1 0.06176(9) -0.3542(2) 0.36185(10) 0.0558(5) Uani d . . Na
O1W 1 0.1429(2) -0.5188(5) 0.3570(3) 0.0810(13) Uani d D . O
H1WA 1 0.1876(15) -0.5134(62) 0.3610(33) 0.080 Uiso d D . H
H1WB 1 0.1333(25) -0.5845(52) 0.3148(24) 0.080 Uiso d D . H
O2W 1 0.0030(3) -0.5425(7) 0.4142(3) 0.128(2) Uani d D . O
H2WA 1 -0.0136(24) -0.5945(57) 0.4580(24) 0.080 Uiso d D . H
H2WB 1 0.0308(24) -0.5005(61) 0.4555(27) 0.080 Uiso d D . H
O3W 1 0 -0.4850(7) 0.25 0.086(2) Uani d SD . O
H3W 1 -0.0102(27) -0.5161(58) 0.3017(21) 0.080 Uiso d D . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Na Na 0.0362 0.0249 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N Fe1 C3 . . 177.3(2) yes
N Fe1 C4 . . 92.7(2) yes
C3 Fe1 C4 . . 84.7(2) yes
N Fe1 C5 . . 97.0(2) yes
C3 Fe1 C5 . . 85.6(2) yes
C4 Fe1 C5 . . 170.1(2) yes
N Fe1 C1 . . 94.9(2) yes
C3 Fe1 C1 . . 85.8(2) yes
C4 Fe1 C1 . . 89.0(2) yes
C5 Fe1 C1 . . 88.3(2) yes
N Fe1 C2 . . 94.5(2) yes
C3 Fe1 C2 . . 84.9(2) yes
C4 Fe1 C2 . . 91.1(2) yes
C5 Fe1 C2 . . 90.0(2) yes
C1 Fe1 C2 . . 170.6(2) yes
O N Fe1 . . 176.7(4) yes
N1 C1 Fe1 . . 179.4(4) ?
N2 C2 Fe1 . . 179.3(5) ?
N3 C3 Fe1 . . 179.7(5) ?
N4 C4 Fe1 . . 177.9(4) ?
N5 C5 Fe1 . . 178.5(4) ?
C1 N1 Na1 . . 163.6(4) ?
C14B N12 C12B . . 112.5(7) ?
C14B N12 C15B . . 111.3(6) ?
C12B N12 C15B . . 109.2(8) ?
C13A N12 C14A . . 111.6(10) ?
C13A N12 C15A . . 114.0(10) ?
C14A N12 C15A . . 108.0(9) ?
C13A N12 C12A . . 111.3(11) ?
C14A N12 C12A . . 105.8(11) ?
C15A N12 C12A . . 105.6(11) ?
C14B N12 C13B . . 106.3(6) ?
C12B N12 C13B . . 109.7(8) ?
C15B N12 C13B . . 107.6(6) ?
O1W Na1 O2W . . 87.9(2) yes
O1W Na1 N1 . . 102.1(2) yes
O2W Na1 N1 . . 155.1(2) yes
O1W Na1 N2 . 6_556 100.6(2) yes
O2W Na1 N2 . 6_556 102.3(2) yes
N1 Na1 N2 . 6_556 98.1(2) yes
O1W Na1 O3W . . 91.5(2) yes
O2W Na1 O3W . . 71.9(2) yes
N1 Na1 O3W . . 85.0(2) yes
N2 Na1 O3W 6_556 . 166.50(15) yes
Na1 O3W Na1 . 2 124.9(3) yes
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
Fe1 N . 1.654(4) yes
Fe1 C3 . 1.929(5) yes
Fe1 C4 . 1.930(5) yes
Fe1 C5 . 1.935(5) yes
Fe1 C1 . 1.936(5) yes
Fe1 C2 . 1.947(5) yes
N O . 1.128(5) yes
C1 N1 . 1.140(5) yes
N3 C3 . 1.144(6) yes
C2 N2 . 1.133(5) yes
N2 Na1 6 2.474(5) yes
C4 N4 . 1.142(6) yes
C5 N5 . 1.144(6) yes
N1 Na1 . 2.406(4) yes
N12 C13A . 1.442(14) ?
N12 C14B . 1.469(10) ?
N12 C12B . 1.474(11) ?
N12 C15B . 1.479(10) ?
N12 C14A . 1.493(15) ?
N12 C15A . 1.507(14) ?
N12 C12A . 1.52(2) ?
N12 C13B . 1.529(10) ?
Na1 O1W . 2.302(4) yes
Na1 O2W . 2.344(5) yes
Na1 N2 6_556 2.474(5) yes
Na1 O3W . 2.574(4) yes
O3W Na1 2 2.574(4) yes
