#------------------------------------------------------------------------------
#$Date: 2010-05-13 20:58:46 +0300 (Thu, 13 May 2010) $
#$Revision: 1167 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/7201190.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_7201190
loop_
_publ_author_name
'Kutasi, Anna M.'
'Turner, David R.'
'Jensen, Paul'
'Moubaraki, Boujemaa'
'Batten, Stuart R.'
'Murray, Keith S.'
_publ_section_title
;
 Coordination polymers of nitrocyanamide, O2NNCN−: synthesis,
 structure and magnetism
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2089
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C6 H8 Fe N8 O6, 2 (H2 O)'
_chemical_formula_sum            'C6 H12 Fe N8 O8'
_chemical_formula_weight         380.09
_chemical_name_common            {[Fe(CAN)2(pyz)(H2O)2].2H2O}
_chemical_name_systematic
;
catena[bis(aqua)bis(nitrocyanamide)(pyrazine)iron(II)] dihydrate
;
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.404(1)
_cell_angle_beta                 90.408(1)
_cell_angle_gamma                108.002(1)
_cell_formula_units_Z            1
_cell_length_a                   6.7652(1)
_cell_length_b                   7.1822(1)
_cell_length_c                   8.6218(2)
_cell_measurement_reflns_used    6688
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.69
_cell_volume                     372.961(12)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6688
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  0.8736
_exptl_absorpt_correction_T_min  0.5912
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             194
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0244
_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/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0579
_reflns_number_gt                1552
_reflns_number_total             1706
_reflns_threshold_expression     >2sigma(I)
_[local]_cod_data_source_file    b905970a.txt
_[local]_cod_data_source_block   2Fe
_[local]_cod_cif_authors_sg_H-M  P-1
_cod_original_cell_volume        372.961(11)
_cod_database_code               7201190
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.5000 0.5000 0.01175(10) Uani 1 2 d S . .
O1 O 0.17946(16) 0.41483(17) 0.51096(15) 0.0175(2) Uani 1 1 d . . .
O2 O 0.06931(17) 0.45923(19) 0.81240(14) 0.0226(2) Uani 1 1 d . . .
N1 N 0.50397(18) 0.80725(17) 0.50045(14) 0.0138(2) Uani 1 1 d . . .
O3 O 0.19300(19) -0.09039(16) -0.03919(14) 0.0277(3) Uani 1 1 d . . .
N2 N 0.43115(19) 0.37130(17) 0.23587(15) 0.0173(3) Uani 1 1 d . . .
N4 N 0.19846(19) 0.01923(19) -0.12542(15) 0.0203(3) Uani 1 1 d . . .
N3 N 0.2883(2) 0.22991(19) -0.06024(15) 0.0210(3) Uani 1 1 d . . .
O4 O 0.12285(19) -0.05288(18) -0.27225(14) 0.0320(3) Uani 1 1 d . . .
C11 C 0.6301(2) 0.9874(2) 0.60980(17) 0.0158(3) Uani 1 1 d . . .
H11 H 0.7250 0.9839 0.6897 0.019 Uiso 1 1 calc R . .
C10 C 0.3739(2) 0.8214(2) 0.39024(17) 0.0154(3) Uani 1 1 d . . .
H10 H 0.2821 0.6969 0.3101 0.018 Uiso 1 1 calc R . .
C12 C 0.3611(2) 0.2933(2) 0.09853(18) 0.0156(3) Uani 1 1 d . . .
H3 H 0.134(3) 0.424(3) 0.603(3) 0.041(6) Uiso 1 1 d . . .
H4 H 0.095(4) 0.331(4) 0.442(3) 0.042(6) Uiso 1 1 d . . .
H5 H 0.132(4) 0.407(4) 0.851(3) 0.049(7) Uiso 1 1 d . . .
H6 H 0.115(4) 0.587(4) 0.864(3) 0.054(7) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.01463(16) 0.00899(14) 0.01053(16) 0.00233(11) -0.00207(10) 0.00367(10)
O1 0.0157(5) 0.0186(5) 0.0138(6) 0.0022(4) -0.0020(5) 0.0038(4)
O2 0.0221(6) 0.0226(6) 0.0180(6) 0.0040(5) -0.0017(4) 0.0037(5)
N1 0.0166(6) 0.0107(5) 0.0140(6) 0.0043(5) -0.0007(5) 0.0046(4)
O3 0.0395(7) 0.0156(5) 0.0238(6) 0.0046(5) 0.0014(5) 0.0059(5)
N2 0.0238(7) 0.0126(5) 0.0138(6) 0.0036(5) -0.0011(5) 0.0052(5)
N4 0.0204(6) 0.0190(6) 0.0131(7) -0.0004(5) 0.0015(5) 0.0017(5)
N3 0.0280(7) 0.0167(6) 0.0112(6) 0.0028(5) -0.0043(5) -0.0001(5)
O4 0.0342(7) 0.0319(6) 0.0122(6) -0.0028(5) -0.0046(5) -0.0014(5)
C11 0.0179(7) 0.0133(6) 0.0146(7) 0.0036(5) -0.0048(5) 0.0045(5)
C10 0.0176(7) 0.0112(6) 0.0143(7) 0.0021(5) -0.0037(5) 0.0031(5)
C12 0.0172(7) 0.0124(6) 0.0170(8) 0.0057(6) 0.0022(6) 0.0040(5)
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'
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
_geom_angle_publ_flag
O1 Fe1 O1 180.0 2_666 . ?
O1 Fe1 N2 92.38(5) 2_666 . ?
O1 Fe1 N2 87.62(5) . . ?
O1 Fe1 N2 87.62(5) 2_666 2_666 ?
O1 Fe1 N2 92.38(5) . 2_666 ?
N2 Fe1 N2 180.0 . 2_666 ?
O1 Fe1 N1 89.90(4) 2_666 2_666 ?
O1 Fe1 N1 90.10(4) . 2_666 ?
N2 Fe1 N1 89.21(4) . 2_666 ?
N2 Fe1 N1 90.79(4) 2_666 2_666 ?
O1 Fe1 N1 90.10(4) 2_666 . ?
O1 Fe1 N1 89.90(4) . . ?
N2 Fe1 N1 90.79(4) . . ?
N2 Fe1 N1 89.21(4) 2_666 . ?
N1 Fe1 N1 180.0 2_666 . ?
Fe1 O1 H3 119.4(15) . . ?
Fe1 O1 H4 125.8(17) . . ?
H3 O1 H4 109(2) . . ?
H5 O2 H6 108(2) . . ?
C11 N1 C10 116.59(11) . . ?
C11 N1 Fe1 122.92(9) . . ?
C10 N1 Fe1 120.48(9) . . ?
C12 N2 Fe1 169.02(11) . . ?
O4 N4 O3 123.45(12) . . ?
O4 N4 N3 115.83(12) . . ?
O3 N4 N3 120.72(12) . . ?
C12 N3 N4 111.55(11) . . ?
N1 C11 C10 121.77(12) . 2_676 ?
N1 C11 H11 119.1 . . ?
C10 C11 H11 119.1 2_676 . ?
N1 C10 C11 121.65(12) . 2_676 ?
N1 C10 H10 119.2 . . ?
C11 C10 H10 119.2 2_676 . ?
N2 C12 N3 172.11(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.0753(10) 2_666 ?
Fe1 O1 2.0753(10) . ?
Fe1 N2 2.1395(12) . ?
Fe1 N2 2.1395(12) 2_666 ?
Fe1 N1 2.1973(10) 2_666 ?
Fe1 N1 2.1973(11) . ?
O1 H3 0.84(2) . ?
O1 H4 0.77(2) . ?
O2 H5 0.78(2) . ?
O2 H6 0.83(3) . ?
N1 C11 1.3367(18) . ?
N1 C10 1.3400(17) . ?
O3 N4 1.2431(17) . ?
N2 C12 1.1522(18) . ?
N4 O4 1.2344(16) . ?
N4 N3 1.3552(17) . ?
N3 C12 1.3272(19) . ?
C11 C10 1.3815(18) 2_676 ?
C11 H11 0.9500 . ?
C10 C11 1.3815(18) 2_676 ?
C10 H10 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H3 O2 0.84(2) 1.81(2) 2.6523(16) 173(2) .
O1 H4 O4 0.77(2) 2.12(2) 2.8767(16) 168(2) 2
O2 H5 N3 0.78(2) 2.19(3) 2.9667(18) 174(2) 1_556
O2 H6 O3 0.83(3) 2.07(3) 2.8918(16) 170(2) 1_566