#------------------------------------------------------------------------------
#$Date: 2019-11-25 00:55:44 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239818 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/02/4350263.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_4350263
loop_
_publ_author_name
'Galet, Ana'
'Muñoz, M Carmen'
'Real, José Antonio'
_publ_section_title
;
 {Fe(3CNpy)2[Cu(3CNpy)(mu-CN)2]2}: a one-dimensional cyanide-based
 spin-crossover coordination polymer.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4583
_journal_page_last               4585
_journal_paper_doi               10.1021/ic060247i
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C28 H16 Cu2 Fe N12'
_chemical_formula_weight         703.46
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                73.765(2)
_cell_angle_beta                 84.770(2)
_cell_angle_gamma                80.681(2)
_cell_formula_units_Z            1
_cell_length_a                   6.8490(3)
_cell_length_b                   7.7800(4)
_cell_length_c                   13.7260(8)
_cell_measurement_temperature    130(2)
_cell_volume                     692.15(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5444
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    2.083
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.102
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0545
_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)+(0.0502P)²+1.8845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                2231
_reflns_number_total             3087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060247isi20060214_050238.cif
_cod_data_source_block           130_K
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4350263
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
Fe Fe 1.0000 0.0000 0.0000 0.0199(2) Uani 1 2 d S
Cu Cu 0.43163(8) 0.39568(8) 0.08271(4) 0.02434(18) Uani 1 1 d .
N2 N 0.8004(5) 0.2171(5) -0.0256(3) 0.0233(8) Uani 1 1 d .
C12 C 0.7571(7) 0.2137(7) 0.3590(4) 0.0284(10) Uani 1 1 d .
N3 N 1.1731(5) 0.1289(5) 0.0519(3) 0.0243(8) Uani 1 1 d .
N1 N 0.8806(5) -0.0923(5) 0.1410(3) 0.0242(8) Uani 1 1 d .
N5 N 0.6350(6) 0.3546(5) 0.1928(3) 0.0261(8) Uani 1 1 d .
C13 C 0.6111(7) 0.2513(6) 0.2887(4) 0.0255(10) Uani 1 1 d .
H13 H 0.4932 0.2035 0.3085 0.034(5) Uiso 1 1 calc R
C10 C 0.9554(7) 0.3931(6) 0.2324(4) 0.0284(10) Uani 1 1 d .
H10 H 1.0711 0.4438 0.2105 0.034(5) Uiso 1 1 calc R
C1 C 0.6862(7) -0.0981(7) 0.1614(4) 0.0315(11) Uani 1 1 d .
H1 H 0.5999 -0.0505 0.1088 0.034(5) Uiso 1 1 calc R
C11 C 0.9333(7) 0.2861(7) 0.3299(4) 0.0302(11) Uani 1 1 d .
H11 H 1.0334 0.2627 0.3753 0.034(5) Uiso 1 1 calc R
C8 C 0.6895(7) 0.3483(6) -0.0388(4) 0.0239(10) Uani 1 1 d .
C4 C 0.9353(8) -0.2449(7) 0.3151(4) 0.0309(11) Uani 1 1 d .
C5 C 1.0028(8) -0.1634(7) 0.2178(4) 0.0309(11) Uani 1 1 d .
H5 H 1.1376 -0.1575 0.2050 0.034(5) Uiso 1 1 calc R
C9 C 0.8043(7) 0.4242(6) 0.1676(4) 0.0278(10) Uani 1 1 d .
H9 H 0.8209 0.4983 0.1022 0.034(5) Uiso 1 1 calc R
N4 N 1.2049(8) -0.4101(8) 0.4424(4) 0.0572(15) Uani 1 1 d .
C3 C 0.7334(8) -0.2517(7) 0.3373(4) 0.0346(12) Uani 1 1 d .
H3 H 0.6848 -0.3068 0.4021 0.034(5) Uiso 1 1 calc R
C2 C 0.6096(8) -0.1727(7) 0.2582(4) 0.0381(13) Uani 1 1 d .
H2 H 0.4734 -0.1694 0.2700 0.034(5) Uiso 1 1 calc R
C14 C 0.7286(8) 0.0983(7) 0.4596(4) 0.0359(12) Uani 1 1 d .
C6 C 1.0814(9) -0.3352(8) 0.3884(4) 0.0402(13) Uani 1 1 d .
N6 N 0.7106(7) 0.0044(8) 0.5397(4) 0.0539(14) Uani 1 1 d .
C7 C 0.2739(7) 0.2166(6) 0.0741(4) 0.0239(10) Uani 1 1 d .
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'
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
N3 Fe N3 180.0(2) 2_755 .
N3 Fe N2 90.54(15) 2_755 .
N3 Fe N2 89.46(15) . .
N3 Fe N2 89.46(15) 2_755 2_755
N3 Fe N2 90.54(15) . 2_755
N2 Fe N2 180.0(3) . 2_755
N3 Fe N1 89.61(16) 2_755 .
N3 Fe N1 90.39(16) . .
N2 Fe N1 91.02(15) . .
N2 Fe N1 88.98(15) 2_755 .
N3 Fe N1 90.39(16) 2_755 2_755
N3 Fe N1 89.61(16) . 2_755
N2 Fe N1 88.98(15) . 2_755
N2 Fe N1 91.02(15) 2_755 2_755
N1 Fe N1 180.00(13) . 2_755
C7 Cu C8 117.01(18) . 2_665
C7 Cu N5 124.03(18) . .
C8 Cu N5 111.59(17) 2_665 .
C7 Cu C8 99.10(17) . .
C8 Cu C8 107.52(15) 2_665 .
N5 Cu C8 91.06(16) . .
C7 Cu Cu 119.42(14) . 2_665
C8 Cu Cu 60.87(13) 2_665 2_665
N5 Cu Cu 107.31(11) . 2_665
C8 Cu Cu 46.66(12) . 2_665
C8 N2 Fe 176.7(4) . .
C13 C12 C11 119.2(4) . .
C13 C12 C14 120.5(4) . .
C11 C12 C14 120.3(5) . .
C7 N3 Fe 173.8(4) 1_655 .
C1 N1 C5 118.0(4) . .
C1 N1 Fe 123.4(3) . .
C5 N1 Fe 118.4(3) . .
C9 N5 C13 117.2(4) . .
C9 N5 Cu 119.4(3) . .
C13 N5 Cu 123.2(3) . .
N5 C13 C12 122.2(4) . .
N5 C13 H13 118.9 . .
C12 C13 H13 118.9 . .
C11 C10 C9 119.1(4) . .
C11 C10 H10 120.5 . .
C9 C10 H10 120.5 . .
N1 C1 C2 122.2(5) . .
N1 C1 H1 118.9 . .
C2 C1 H1 118.9 . .
C10 C11 C12 118.3(5) . .
C10 C11 H11 120.9 . .
C12 C11 H11 120.9 . .
N2 C8 Cu 163.0(4) . 2_665
N2 C8 Cu 122.1(4) . .
Cu C8 Cu 72.48(15) 2_665 .
C5 C4 C3 120.2(5) . .
C5 C4 C6 117.5(5) . .
C3 C4 C6 122.1(5) . .
N1 C5 C4 122.3(5) . .
N1 C5 H5 118.9 . .
C4 C5 H5 118.9 . .
N5 C9 C10 124.1(5) . .
N5 C9 H9 118.0 . .
C10 C9 H9 118.0 . .
C2 C3 C4 116.6(5) . .
C2 C3 H3 121.7 . .
C4 C3 H3 121.7 . .
C3 C2 C1 120.7(5) . .
C3 C2 H2 119.7 . .
C1 C2 H2 119.7 . .
N6 C14 C12 178.3(6) . .
N4 C6 C4 176.0(7) . .
N3 C7 Cu 167.9(4) 1_455 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe N3 1.963(4) 2_755
Fe N3 1.963(4) .
Fe N2 1.963(4) .
Fe N2 1.963(4) 2_755
Fe N1 2.014(4) .
Fe N1 2.014(4) 2_755
Cu C7 1.930(5) .
Cu C8 1.976(5) 2_665
Cu N5 2.072(4) .
Cu C8 2.373(5) .
Cu Cu 2.5906(11) 2_665
N2 C8 1.150(6) .
C12 C13 1.394(7) .
C12 C11 1.393(7) .
C12 C14 1.437(7) .
N3 C7 1.159(6) 1_655
N1 C1 1.341(6) .
N1 C5 1.342(6) .
N5 C9 1.335(6) .
N5 C13 1.348(6) .
C13 H13 0.9300 .
C10 C11 1.374(7) .
C10 C9 1.373(7) .
C10 H10 0.9300 .
C1 C2 1.384(7) .
C1 H1 0.9300 .
C11 H11 0.9300 .
C8 Cu 1.976(5) 2_665
C4 C5 1.382(7) .
C4 C3 1.395(7) .
C4 C6 1.438(7) .
C5 H5 0.9300 .
C9 H9 0.9300 .
N4 C6 1.148(7) .
C3 C2 1.379(8) .
C3 H3 0.9300 .
C2 H2 0.9300 .
C14 N6 1.146(7) .
C7 N3 1.159(6) 1_455
