#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:21:52 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179057 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/19/4301900.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_4301900
loop_
_publ_author_name
'Gloria Agustí'
'M. Carmen Muñoz'
'Ana B. Gaspar'
'José A. Real'
_publ_section_title
;
Spin-Crossover Behavior in Cyanide-Bridged Iron(II)-Copper(I) Bimetallic
1-3D Metal-Organic Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3371
_journal_page_last               3381
_journal_paper_doi               10.1021/ic8010458
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C24 H16 Cu2 Fe I4 N8'
_chemical_formula_weight         1106.98
_chemical_name_systematic
;
 ?
;
_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                92.575(4)
_cell_angle_beta                 92.975(3)
_cell_angle_gamma                92.992(2)
_cell_formula_units_Z            1
_cell_length_a                   8.3870(6)
_cell_length_b                   8.6050(7)
_cell_length_c                   10.4070(9)
_cell_measurement_temperature    293(2)
_cell_volume                     748.18(10)
_computing_cell_refinement       'HKL DENZO'
_computing_data_collection       COLLECT
_computing_data_reduction        'HKL DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4229
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    6.043
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.642
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0556
_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)+(0.0740P)²+3.8312P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1553
_reflns_number_gt                2390
_reflns_number_total             3349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8010458_si_001_9.cif
_cod_data_source_block           Compound5-293K
_cod_database_code               4301900
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
Fe Fe 0.5000 0.0000 0.5000 0.0337(4) Uani 1 2 d S . .
Cu Cu 0.02314(13) 0.28333(12) 0.67687(11) 0.0428(3) Uani 1 1 d . . .
I1 I 0.66023(8) 0.21087(7) -0.03906(6) 0.0463(2) Uani 1 1 d . . .
I2 I -0.16924(8) 0.77234(7) 1.03865(6) 0.0469(2) Uani 1 1 d . . .
N1 N 0.5068(9) 0.1834(8) 0.3499(7) 0.0395(16) Uani 1 1 d . . .
N2 N 0.3226(9) 0.1278(8) 0.5986(8) 0.0425(17) Uani 1 1 d . . .
N3 N 0.6917(9) 0.1308(8) 0.6125(7) 0.0415(17) Uani 1 1 d . . .
N4 N 0.0135(9) 0.5203(8) 0.7185(7) 0.0417(17) Uani 1 1 d . . .
C1 C 0.4702(13) 0.3309(11) 0.3770(9) 0.047(2) Uani 1 1 d . . .
H1 H 0.4326 0.3537 0.4579 0.057(11) Uiso 1 1 calc R . .
C2 C 0.4836(14) 0.4488(10) 0.2962(10) 0.053(3) Uani 1 1 d . . .
H2 H 0.4541 0.5481 0.3205 0.057(11) Uiso 1 1 calc R . .
C3 C 0.5425(13) 0.4183(10) 0.1757(9) 0.047(2) Uani 1 1 d . . .
H3 H 0.5549 0.4971 0.1181 0.057(11) Uiso 1 1 calc R . .
C4 C 0.5825(11) 0.2666(10) 0.1433(8) 0.0374(18) Uani 1 1 d . . .
C5 C 0.5621(11) 0.1535(10) 0.2337(8) 0.0385(19) Uani 1 1 d . . .
H5 H 0.5881 0.0523 0.2120 0.057(11) Uiso 1 1 calc R . .
C6 C 0.2187(11) 0.1920(10) 0.6321(9) 0.0392(19) Uani 1 1 d . . .
C7 C 0.8101(11) 0.1886(10) 0.6469(9) 0.040(2) Uani 1 1 d . . .
C8 C 0.0596(12) 0.6323(11) 0.6422(9) 0.048(2) Uani 1 1 d . . .
H8 H 0.1107 0.6039 0.5681 0.057(11) Uiso 1 1 calc R . .
C9 C 0.0362(15) 0.7876(11) 0.6664(10) 0.058(3) Uani 1 1 d . . .
H9 H 0.0677 0.8608 0.6084 0.057(11) Uiso 1 1 calc R . .
C10 C -0.0343(13) 0.8337(10) 0.7776(9) 0.048(2) Uani 1 1 d . . .
H10 H -0.0512 0.9380 0.7967 0.057(11) Uiso 1 1 calc R . .
C11 C -0.0791(10) 0.7192(9) 0.8597(8) 0.0353(17) Uani 1 1 d . . .
C12 C -0.0566(11) 0.5657(9) 0.8265(9) 0.0389(19) Uani 1 1 d . . .
H12 H -0.0914 0.4898 0.8811 0.057(11) Uiso 1 1 calc R . .
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'
I I -0.4742 1.8119 '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'
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
N1 Fe N1 180.000(1) . 2_656 ?
N2 Fe N1 90.5(3) 2_656 . ?
N2 Fe N1 89.5(3) . . ?
N2 Fe N1 89.5(3) 2_656 2_656 ?
N2 Fe N1 90.5(3) . 2_656 ?
N3 Fe N1 90.3(3) 2_656 . ?
N3 Fe N1 89.7(3) . . ?
N3 Fe N1 89.7(3) 2_656 2_656 ?
N3 Fe N1 90.3(3) . 2_656 ?
N2 Fe N2 180.000(1) 2_656 . ?
N2 Fe N3 90.8(3) 2_656 2_656 ?
N2 Fe N3 89.2(3) . 2_656 ?
N2 Fe N3 89.2(3) 2_656 . ?
N2 Fe N3 90.8(3) . . ?
N3 Fe N3 180.0(3) 2_656 . ?
C6 Cu N4 121.7(3) . . ?
C7 Cu N4 110.2(3) 1_455 . ?
C6 Cu C7 126.2(4) . 1_455 ?
C5 N1 C1 116.4(7) . . ?
C5 N1 Fe 121.4(6) . . ?
C1 N1 Fe 121.9(6) . . ?
C6 N2 Fe 169.6(8) . . ?
C7 N3 Fe 164.0(7) . . ?
C8 N4 C12 116.6(7) . . ?
C8 N4 Cu 125.3(6) . . ?
C12 N4 Cu 117.8(6) . . ?
N1 C1 C2 125.2(9) . . ?
N1 C1 H1 117.4 . . ?
C2 C1 H1 117.4 . . ?
C1 C2 C3 118.5(8) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C2 C3 C4 118.4(8) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 118.3(8) . . ?
C5 C4 I1 121.4(6) . . ?
C3 C4 I1 120.2(6) . . ?
N1 C5 C4 123.2(8) . . ?
N1 C5 H5 118.4 . . ?
C4 C5 H5 118.4 . . ?
N2 C6 Cu 172.7(8) . . ?
N3 C7 Cu 170.5(8) . 1_655 ?
N4 C8 C9 123.8(9) . . ?
N4 C8 H8 118.1 . . ?
C9 C8 H8 118.1 . . ?
C8 C9 C10 119.4(9) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C9 C10 C11 117.6(8) . . ?
C9 C10 H10 121.2 . . ?
C11 C10 H10 121.2 . . ?
C12 C11 C10 119.6(8) . . ?
C12 C11 I2 118.3(6) . . ?
C10 C11 I2 122.0(6) . . ?
N4 C12 C11 123.0(8) . . ?
N4 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
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
Fe N1 2.270(7) . ?
Fe N1 2.270(7) 2_656 ?
Fe N2 2.168(7) 2_656 ?
Fe N2 2.168(7) . ?
Fe N3 2.172(7) 2_656 ?
Fe N3 2.172(7) . ?
Cu N4 2.072(7) . ?
Cu C6 1.925(9) . ?
Cu C7 1.929(10) 1_455 ?
I1 C4 2.083(9) . ?
I2 C11 2.087(9) . ?
N1 C5 1.337(11) . ?
N1 C1 1.342(11) . ?
N2 C6 1.119(11) . ?
N3 C7 1.122(11) . ?
N4 C8 1.330(12) . ?
N4 C12 1.347(11) . ?
C1 C2 1.351(13) . ?
C1 H1 0.9300 . ?
C2 C3 1.390(13) . ?
C2 H2 0.9300 . ?
C3 C4 1.396(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(12) . ?
C5 H5 0.9300 . ?
C7 Cu 1.929(9) 1_655 ?
C8 C9 1.375(14) . ?
C8 H8 0.9300 . ?
C9 C10 1.379(14) . ?
C9 H9 0.9300 . ?
C10 C11 1.382(12) . ?
C10 H10 0.9300 . ?
C11 C12 1.375(11) . ?
C12 H12 0.9300 . ?
