#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:50:02 +0100 (lun 21 de mar de 2016) $
#$Revision: 178794 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/48/4104810.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_4104810
loop_
_publ_author_name
'Peter D. Southon'
'Lang Liu'
'Elizabeth A. Fellows'
'David J. Price'
'Gregory J. Halder'
'Karena W. Chapman'
'Boujemaa Moubaraki'
'Keith S. Murray'
'Jean-François Létard'
'Cameron J. Kepert'
_publ_contact_author_address
; 
School of Chemistry
University of Sydney
NSW 2006
Australia
;
_publ_contact_author_email       c.kepert@chem.usyd.edu.au
_publ_contact_author_fax         +61-2-9351-3329
_publ_contact_author_name        'Prof. Cameron J. Kepert'
_publ_contact_author_phone       +61-2-9351-5741
_publ_section_title
;
 Dynamic Interplay between Spin-Crossover and Host-Guest Function in a
 Nanoporous Metal-Organic Framework Material
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10998
_journal_page_last               11009
_journal_paper_doi               10.1021/ja902187d
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C8 H8 Fe N6 Ni O2'
_chemical_formula_weight         334.76
_chemical_name_common            '[Fe(pz)Ni(CN)4].2H2O'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           47
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2'
_symmetry_space_group_name_H-M   'P m m 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                90.00
_cell_formula_units_Z            1
_cell_length_a                   7.2666(3)
_cell_length_b                   7.2696(3)
_cell_length_c                   7.2421(3)
_cell_measurement_reflns_used    1599
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      29.9535
_cell_measurement_theta_min      2.802
_cell_volume                     382.57(3)
_computing_cell_refinement       'SAINT Ver. 7.23A  (Bruker-AXS, 2005)'
_computing_data_collection       'APEX2 Ver. 2.1-3 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT Ver. 7.23A'
_computing_molecular_graphics    'XPMA/ZORTEP, WebLab Viewer 3.7'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker-Nonius FR591 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3451
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         2.80
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.180
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            red-yellow
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             168
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.016
_refine_diff_density_max         1.422
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         688
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0449P)²+0.7689P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                526
_reflns_number_total             688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja902187d_si_001_4.cif
_cod_data_source_block           1.2H2O(300t)
_cod_database_code               4104810
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'-x, -y, -z'
'x, y, -z'
'-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
Ni1 Ni 0.5000 0.5000 0.0000 0.0220(3) Uani 1 8 d S
Fe1 Fe 0.0000 0.0000 0.0000 0.0192(3) Uani 1 8 d S
O11 O 0.5000 0.0000 0.399(11) 0.176(14) Uiso 0.272(4) 4 d SP
O12 O 0.5000 0.401(5) 0.5000 0.176(14) Uiso 0.53(2) 4 d SP
O13 O 0.5000 0.5000 0.323(13) 0.176(14) Uiso 0.19(2) 4 d SP
N1 N 0.2051(14) 0.2088(11) 0.0000 0.0327(10) Uani 1 2 d S
N2 N 0.0000 0.0000 0.3073(8) 0.0336(14) Uani 1 4 d S
C1 C 0.3243(15) 0.3120(16) 0.0000 0.0253(10) Uani 1 2 d S
C2 C 0.0000 0.1544(11) 0.4031(12) 0.075(3) Uani 1 2 d S
H2 H 0.0000 0.2661 0.3406 0.090 Uiso 1 2 calc SR
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
Ni1 0.0102(15) 0.0122(17) 0.0438(7) 0.000 0.000 0.000
Fe1 0.0078(16) 0.018(2) 0.0322(6) 0.000 0.000 0.000
N1 0.044(4) 0.005(2) 0.050(2) 0.000 0.000 -0.0054(14)
N2 0.050(7) 0.015(5) 0.036(3) 0.000 0.000 0.000
C1 0.020(4) 0.013(3) 0.043(2) 0.000 0.000 0.0038(19)
C2 0.143(10) 0.025(3) 0.055(4) -0.001(3) 0.000 0.000
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'
Ni Ni 0.3393 1.1124 '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
C1 Ni1 C1 180.000(1) 5_665 .
C1 Ni1 C1 93.9(9) 5_665 7_655
C1 Ni1 C1 86.1(9) . 7_655
C1 Ni1 C1 86.1(9) 5_665 3_565
C1 Ni1 C1 93.9(9) . 3_565
C1 Ni1 C1 180.000(1) 7_655 3_565
C1 Ni1 O13 90.000(3) 5_665 .
C1 Ni1 O13 90.000(3) . .
C1 Ni1 O13 90.000(3) 7_655 .
C1 Ni1 O13 90.000(3) 3_565 .
C1 Ni1 O13 90.000(3) 5_665 5_665
C1 Ni1 O13 90.000(3) . 5_665
C1 Ni1 O13 90.000(3) 7_655 5_665
C1 Ni1 O13 90.000(3) 3_565 5_665
O13 Ni1 O13 180.000(2) . 5_665
N1 Fe1 N1 180.0(3) 5 .
N1 Fe1 N1 91.0(6) 5 7
N1 Fe1 N1 89.0(6) . 7
N1 Fe1 N1 89.0(6) 5 3
N1 Fe1 N1 91.0(6) . 3
N1 Fe1 N1 180.0 7 3
N1 Fe1 N2 90.0 5 .
N1 Fe1 N2 90.0 . .
N1 Fe1 N2 90.0 7 .
N1 Fe1 N2 90.0 3 .
N1 Fe1 N2 90.0 5 5
N1 Fe1 N2 90.0 . 5
N1 Fe1 N2 90.0 7 5
N1 Fe1 N2 90.0 3 5
N2 Fe1 N2 180.0 . 5
O12 O12 O13 61(3) 5_666 5_666
O12 O12 O13 61(3) 5_666 .
O13 O12 O13 121(5) 5_666 .
O12 O13 O12 59(5) 5_666 .
O12 O13 Ni1 151(3) 5_666 .
O12 O13 Ni1 151(3) . .
C1 N1 Fe1 175.4(15) . .
C2 N2 C2 116.6(8) . 2
C2 N2 Fe1 121.7(4) . .
C2 N2 Fe1 121.7(4) 2 .
N1 C1 Ni1 173.9(17) . .
N2 C2 C2 121.7(4) . 6_556
N2 C2 H2 119.1 . .
C2 C2 H2 119.1 6_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 C1 1.870(5) 5_665
Ni1 C1 1.870(5) .
Ni1 C1 1.870(5) 7_655
Ni1 C1 1.870(5) 3_565
Ni1 O13 2.34(10) .
Ni1 O13 2.34(10) 5_665
Fe1 N1 2.128(4) 5
Fe1 N1 2.128(4) .
Fe1 N1 2.128(4) 7
Fe1 N1 2.128(4) 3
Fe1 N2 2.226(6) .
Fe1 N2 2.226(6) 5
O11 O11 1.46(16) 5_656
O12 O12 1.44(8) 5_666
O12 O13 1.47(8) 5_666
O12 O13 1.47(8) .
O13 O12 1.47(8) 5_666
N1 C1 1.145(7) .
N2 C2 1.319(8) .
N2 C2 1.319(8) 2
C2 C2 1.403(17) 6_556
C2 H2 0.9300 .
