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#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/27/7012793.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_7012793
loop_
_publ_author_name
'Sugiyarto, Kristian H.'
'McHale, Wendy-Anne'
'Craig, Donald C.'
'Rae, A. David'
'Scudder, Marcia L.'
'Goodwin, Harold A.'
_publ_section_title
;
 Spin transition centres linked by the nitroprusside ion. The
 cooperative transition in bis(2,6-bis(pyrazol-3-yl)pyridine)iron(ii)
 nitroprusside
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              2443
_journal_paper_doi               10.1039/b301218b
_journal_year                    2003
_chemical_formula_moiety         'C22 H18 Fe N10 2+,C5 Fe N6 O 2-'
_chemical_formula_sum            'C27 H18 Fe2 N16 O'
_chemical_formula_weight         694.2
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_atom_type_scat_source
'International Tables for X-ray Crystallography, Vol. IV'
_audit_creation_method           'RAELSPUB and manual entry'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.346(3)
_cell_length_b                   13.346(3)
_cell_length_c                   17.273(5)
_cell_measurement_reflns_used    10
_cell_measurement_temperature    294
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9
_cell_volume                     3076.6(13)
_computing_cell_refinement       'CAD4 Version 5.0, 1989'
_computing_data_collection       'CAD4 Version 5.0, 1989'
_computing_data_reduction        'Local program'
_computing_molecular_graphics    'ORTEP-II, (Johnson, 1976)'
_computing_publication_material  'Local programs'
_computing_structure_refinement  'RAELS, (Rae, 1989)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2620
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30min
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(DeMeulenaer & Tompa, 1965)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.50
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408.0
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     112
_refine_ls_number_reflns         875
_refine_ls_R_factor_gt           0.034
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F) + 0.0004F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.041
_reflns_number_gt                875
_reflns_number_total             1361
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b301218b.txt
_cod_data_source_block           C22H18FeN10,C5FeN6O_DHG72_RT
_cod_original_cell_volume        3077(1)
_cod_original_sg_symbol_H-M      'P 4/ncc'
_cod_database_code               7012793
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,y,1/2+z
3 x,1/2-y,1/2+z
4 1/2-x,1/2-y,z
5 y,x,1/2+z
6 1/2-y,x,z
7 y,1/2-x,z
8 1/2-y,1/2-x,1/2+z
9 -x,-y,-z
10 1/2+x,-y,1/2-z
11 -x,1/2+y,1/2-z
12 1/2+x,1/2+y,-z
13 -y,-x,1/2-z
14 1/2+y,-x,-z
15 -y,1/2+x,-z
16 1/2+y,1/2+x,1/2-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_adp_type
_atom_site_type_symbol
_atom_site_occupancy
Fe1 0.7500 0.2500 0.2500 0.0367(2) Uani Fe 1.0
N1 0.8560(2) 0.2904(2) 0.1585(2) 0.0455(7) Uani N 1.0
N2 0.8604(2) 0.3567(2) 0.1002(2) 0.0583(8) Uani N 1.0
N3 0.8635(2) 0.1365(2) 0.2500 0.0461(9) Uani N 1.0
C1 0.9360(4) 0.3355(3) 0.0518(2) 0.074(1) Uani C 1.0
C2 0.9825(3) 0.2518(4) 0.0785(2) 0.075(1) Uani C 1.0
C3 0.9307(3) 0.2250(3) 0.1457(2) 0.0524(9) Uani C 1.0
C4 0.9383(3) 0.1412(3) 0.1986(2) 0.055(1) Uani C 1.0
C5 1.0136(3) 0.0693(4) 0.1978(3) 0.086(2) Uani C 1.0
C6 1.0075(3) -0.0075(3) 0.2500 0.106(3) Uani C 1.0
Fe2 0.25000 0.25000 0.36190(4) 0.0398(2) Uani Fe 1.0
O1Np 0.2748(78) 0.2315(96) 0.2028(3) 0.118(9) Uani O 1.0
N1Np 0.2500 0.2500 0.2669(3) 0.074(2) Uani N 1.0
N2Np 0.2500 0.2500 0.5398(3) 0.072(2) Uani N 1.0
C2Np 0.2500 0.2500 0.4745(4) 0.046(1) Uani C 1.0
N3Np 0.0216(3) 0.2344(3) 0.3788(2) 0.081(1) Uani N 1.0
C3Np 0.1063(3) 0.2390(3) 0.3720(2) 0.0528(9) Uani C 1.0
HN2 0.8134 0.4144 0.0936 0.058 Uani H 1.0
HC1 0.9548 0.3743 0.0045 0.074 Uani H 1.0
HC2 1.0414 0.2168 0.0551 0.075 Uani H 1.0
HC5 1.0704 0.0735 0.1602 0.086 Uani H 1.0
HC6 1.0605 -0.0605 0.2500 0.106 Uani H 1.0
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 87.5(1) 1_555 1_555 4_655 no
N1 Fe1 N1 147.2(1) 1_555 1_555 13_665 no
N1 Fe1 N1 101.7(1) 1_555 1_555 16_545 no
N1 Fe1 N3 73.58(7) 1_555 1_555 1_555 no
N1 Fe1 N3 106.42(7) 1_555 1_555 4_655 no
N1 Fe1 N1 101.7(1) 4_655 1_555 13_665 no
N1 Fe1 N1 147.2(1) 4_655 1_555 16_545 no
N1 Fe1 N3 106.42(7) 4_655 1_555 1_555 no
N1 Fe1 N3 73.58(7) 4_655 1_555 4_655 no
N1 Fe1 N1 87.5(1) 13_665 1_555 16_545 no
N1 Fe1 N3 73.58(7) 13_665 1_555 1_555 no
N1 Fe1 N3 106.42(7) 13_665 1_555 4_655 no
N1 Fe1 N3 106.42(7) 16_545 1_555 1_555 no
N1 Fe1 N3 73.58(7) 16_545 1_555 4_655 no
N3 Fe1 N3 180.00 1_555 1_555 4_655 no
Fe1 N1 C3 116.0(2) 1_555 1_555 1_555 no
Fe1 N3 C4 119.7(2) 1_555 1_555 1_555 no
Fe1 N3 C4 119.7(2) 1_555 1_555 13_665 no
C4 N3 C4 120.7(4) 1_555 1_555 13_665 no
N2 C1 C2 107.8(4) 1_555 1_555 1_555 no
C1 C2 C3 105.4(4) 1_555 1_555 1_555 no
N1 C3 C2 109.7(4) 1_555 1_555 1_555 no
N1 C3 C4 116.8(3) 1_555 1_555 1_555 no
C2 C3 C4 133.4(4) 1_555 1_555 1_555 no
N3 C4 C3 113.7(3) 1_555 1_555 1_555 no
N3 C4 C5 120.9(4) 1_555 1_555 1_555 no
C3 C4 C5 125.3(4) 1_555 1_555 1_555 no
C4 C5 C6 117.8(5) 1_555 1_555 1_555 no
C5 C6 C5 121.7(6) 1_555 1_555 13_665 no
N1Np Fe2 C2Np 180.00 1_555 1_555 1_555 no
N1Np Fe2 C3Np 95.17(9) 1_555 1_555 1_555 no
N1Np Fe2 C3Np 95.17(9) 1_555 1_555 4_555 no
N1Np Fe2 C3Np 95.17(9) 1_555 1_555 6_555 no
N1Np Fe2 C3Np 95.17(9) 1_555 1_555 7_555 no
C2Np Fe2 C3Np 84.83(9) 1_555 1_555 1_555 no
C2Np Fe2 C3Np 84.83(9) 1_555 1_555 4_555 no
C2Np Fe2 C3Np 84.83(9) 1_555 1_555 6_555 no
C2Np Fe2 C3Np 84.83(9) 1_555 1_555 7_555 no
C3Np Fe2 C3Np 169.7(2) 1_555 1_555 4_555 no
C3Np Fe2 C3Np 89.53(2) 1_555 1_555 6_555 no
C3Np Fe2 C3Np 89.53(2) 1_555 1_555 7_555 no
C3Np Fe2 C3Np 89.53(2) 4_555 1_555 6_555 no
C3Np Fe2 C3Np 89.53(2) 4_555 1_555 7_555 no
C3Np Fe2 C3Np 169.7(2) 6_555 1_555 7_555 no
Fe2 N1Np O1Np 159.6(21) 1_555 1_555 1_555 no
Fe2 C2Np N2Np 180.00 1_555 1_555 1_555 no
Fe2 C3Np N3Np 178.5(4) 1_555 1_555 1_555 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.189(3) 1_555 1_555 no
Fe1 N1 2.189(3) 1_555 4_655 no
Fe1 N1 2.189(3) 1_555 13_665 no
Fe1 N1 2.189(3) 1_555 16_545 no
Fe1 N3 2.143(3) 1_555 1_555 no
Fe1 N3 2.143(3) 1_555 4_655 no
N1 C3 1.343(4) 1_555 1_555 no
N2 C1 1.340(5) 1_555 1_555 no
N3 C4 1.337(4) 1_555 1_555 no
N3 C4 1.337(4) 1_555 13_665 no
C1 C2 1.358(6) 1_555 1_555 no
C2 C3 1.397(5) 1_555 1_555 no
C3 C4 1.449(4) 1_555 1_555 no
C4 C5 1.390(5) 1_555 1_555 no
C5 C6 1.367(6) 1_555 1_555 no
C6 C5 1.367(6) 1_555 13_665 no
Fe2 N1Np 1.640(5) 1_555 1_555 no
Fe2 C2Np 1.945(6) 1_555 1_555 no
Fe2 C3Np 1.931(4) 1_555 1_555 no
Fe2 C3Np 1.931(4) 1_555 4_555 no
Fe2 C3Np 1.931(4) 1_555 6_555 no
Fe2 C3Np 1.931(4) 1_555 7_555 no
O1Np N1Np 1.182(18) 1_555 1_555 no
N2Np C2Np 1.129(8) 1_555 1_555 no
N3Np C3Np 1.139(4) 1_555 1_555 no
