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#$Date: 2016-03-22 12:38:38 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178957 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/86/4118649.cif $
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#
# 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_4118649
loop_
_publ_author_name
'Luminita M. Toma'
'Catalina Ruiz-Pérez'
'Jorge Pasán'
'Wolfgang Wernsdorfer'
'Francesc Lloret'
'Miguel Julve'
_publ_contact_author_address
;Laboratorio de Rayos X y Materiales Moleculares
 Dpto. Física Fundamental II. Facultad de Física
 Universidad de La Laguna
 E-38204. La Laguna. Tenerife
 Spain
;
_publ_contact_author_email       caruiz@ull.es
_publ_contact_author_fax         +34922318320
_publ_contact_author_name        'Professor Catalina Ruiz-Pérez'
_publ_contact_author_phone       +34922318300
_publ_section_title
;
 Molecular Engineering To Control the Magnetic Interaction between
 Single-Chain Magnets Assembled in a Two-Dimensional Network
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15265
_journal_page_last               15268
_journal_paper_doi               10.1021/ja307042z
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C44 H40 Co Fe2 N14 O2'
_chemical_formula_weight         967.50
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 113.29(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.048(3)
_cell_length_b                   14.0942(4)
_cell_length_c                   11.9188(4)
_cell_measurement_temperature    293(2)
_cell_volume                     4636.3(9)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    CRYSTALMAKER
_computing_publication_material  'PARST97 (Nardelli, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_sigmaI/netI    0.1043
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17852
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         6.43
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            braun
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       naddels
_exptl_crystal_F_000             1948
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1877
_refine_ls_R_factor_gt           0.1401
_refine_ls_shift/su_max          0.878
_refine_ls_shift/su_mean         0.477
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1985P)²+104.3945P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2975
_refine_ls_wR_factor_ref         0.3246
_reflns_number_gt                3274
_reflns_number_total             5188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307042z_si_002.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        4636.4(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4118649
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Co1 Co 0.0000 0.0000 0.0000 0.0352(5) Uani 1 2 d S
Fe1 Fe -0.13527(5) 0.10490(12) -0.38225(14) 0.0437(5) Uani 1 1 d .
N1 N -0.0520(4) 0.0800(9) -0.1335(10) 0.065(3) Uani 1 1 d .
N1O N 0.0033(10) 0.1828(18) 0.1199(18) 0.130(7) Uani 1 1 d .
N2 N 0.1472(6) -0.1106(12) -0.1238(18) 0.111(5) Uani 1 1 d .
N3 N -0.1173(6) 0.3170(14) -0.373(3) 0.145(10) Uani 1 1 d .
N4 N 0.0555(4) 0.0715(10) -0.0285(10) 0.068(3) Uani 1 1 d .
N11 N -0.1906(4) 0.1127(8) -0.5367(10) 0.059(3) Uani 1 1 d .
N12 N -0.1885(4) 0.1246(9) -0.3243(12) 0.069(3) Uani 1 1 d .
O1 O 0.0020(5) 0.0962(7) 0.1387(8) 0.079(3) Uani 1 1 d .
C1 C -0.0841(4) 0.0912(9) -0.2273(11) 0.051(3) Uani 1 1 d .
C2 C 0.1433(4) -0.0337(11) -0.1108(14) 0.066(4) Uani 1 1 d .
C3 C -0.1240(4) 0.2398(10) -0.3769(15) 0.063(4) Uani 1 1 d .
C4 C 0.0846(4) 0.0880(9) -0.0608(11) 0.052(3) Uani 1 1 d .
C11 C -0.1905(6) 0.1077(12) -0.6514(14) 0.081(5) Uani 1 1 d .
H11 H -0.1609 0.1045 -0.6591 0.097 Uiso 1 1 calc R
C12 C -0.2302(6) 0.1073(15) -0.7501(15) 0.093(5) Uani 1 1 d .
H12 H -0.2286 0.1081 -0.8264 0.111 Uiso 1 1 calc R
C13 C -0.2782(6) 0.1055(13) -0.7408(15) 0.078(4) Uani 1 1 d .
C14 C -0.2789(6) 0.1131(11) -0.6250(13) 0.069(4) Uani 1 1 d .
H14 H -0.3077 0.1150 -0.6132 0.083 Uiso 1 1 calc R
C15 C -0.2354(4) 0.1175(9) -0.5315(16) 0.068(4) Uani 1 1 d .
C16 C -0.2329(5) 0.1251(11) -0.4080(15) 0.066(4) Uani 1 1 d .
C17 C -0.2727(6) 0.1334(13) -0.3800(18) 0.088(5) Uani 1 1 d .
H17 H -0.3036 0.1317 -0.4420 0.106 Uiso 1 1 calc R
C18 C -0.2671(7) 0.1449(13) -0.2554(18) 0.094(5) Uani 1 1 d .
C19 C -0.2196(8) 0.1419(16) -0.166(2) 0.109(6) Uani 1 1 d .
H19 H -0.2136 0.1473 -0.0832 0.131 Uiso 1 1 calc R
C20 C -0.1823(6) 0.1307(14) -0.2031(17) 0.086(5) Uani 1 1 d .
H20 H -0.1510 0.1271 -0.1435 0.104 Uiso 1 1 calc R
C21 C -0.3224(6) 0.108(2) -0.8633(18) 0.129(9) Uani 1 1 d .
H21A H -0.3119 0.0996 -0.9290 0.194 Uiso 1 1 calc R
H21B H -0.3386 0.1680 -0.8722 0.194 Uiso 1 1 calc R
H21C H -0.3443 0.0579 -0.8653 0.194 Uiso 1 1 calc R
C22 C -0.3088(8) 0.1596(18) -0.218(2) 0.124(8) Uani 1 1 d .
H22A H -0.3387 0.1602 -0.2888 0.186 Uiso 1 1 calc R
H22B H -0.3049 0.2190 -0.1755 0.186 Uiso 1 1 calc R
H22C H -0.3095 0.1090 -0.1645 0.186 Uiso 1 1 calc R
C3O C -0.0054(15) 0.367(2) 0.060(3) 0.144(9) Uani 1 1 d .
C5O C 0.0420(15) 0.231(2) 0.140(4) 0.202(15) Uani 1 1 d .
H5O H 0.0728 0.2076 0.1873 0.242 Uiso 1 1 calc R
C2O C -0.0414(17) 0.323(2) 0.060(3) 0.195(16) Uani 1 1 d .
H2O H -0.0701 0.3566 0.0411 0.234 Uiso 1 1 calc R
C1O C -0.0404(14) 0.229(3) 0.085(4) 0.237(16) Uani 1 1 d .
H1O H -0.0683 0.1973 0.0802 0.285 Uiso 1 1 calc R
C4O C 0.0337(15) 0.325(3) 0.082(4) 0.205(15) Uani 1 1 d .
H4O H 0.0576 0.3539 0.0622 0.245 Uiso 1 1 calc R
C6O C -0.0144(15) 0.476(2) 0.029(3) 0.198(14) Uani 1 1 d .
H6O1 H -0.0483 0.4839 -0.0249 0.237 Uiso 1 1 calc R
H6O2 H -0.0093 0.5093 0.1039 0.237 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'
Co Co 0.3494 0.9721 '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'
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'
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
N1 Co1 N1 180.0(8) 5 .
N1 Co1 N4 88.8(5) 5 .
N1 Co1 N4 91.2(5) . .
N1 Co1 N4 91.2(5) 5 5
N1 Co1 N4 88.8(5) . 5
N4 Co1 N4 180.0(8) . 5
N1 Co1 O1 88.2(5) 5 .
N1 Co1 O1 91.8(5) . .
N4 Co1 O1 92.3(5) . .
N4 Co1 O1 87.7(5) 5 .
N1 Co1 O1 91.8(5) 5 5
N1 Co1 O1 88.2(5) . 5
N4 Co1 O1 87.7(5) . 5
N4 Co1 O1 92.3(5) 5 5
O1 Co1 O1 180.0(7) . 5
C1 Fe1 C4 83.1(5) . 2_554
C1 Fe1 C3 90.2(6) . .
C4 Fe1 C3 88.9(5) 2_554 .
C1 Fe1 N11 175.6(5) . .
C4 Fe1 N11 100.1(5) 2_554 .
C3 Fe1 N11 92.8(5) . .
C1 Fe1 C2 88.8(6) . 2_554
C4 Fe1 C2 87.9(6) 2_554 2_554
C3 Fe1 C2 176.7(5) . 2_554
N11 Fe1 C2 88.3(5) . 2_554
C1 Fe1 N12 97.5(5) . .
C4 Fe1 N12 179.1(5) 2_554 .
C3 Fe1 N12 90.4(5) . .
N11 Fe1 N12 79.4(5) . .
C2 Fe1 N12 92.9(6) 2_554 .
C1 N1 Co1 154.2(11) . .
O1 N1O C5O 125(3) . .
O1 N1O C1O 115(3) . .
C5O N1O C1O 120(3) . .
C4 N4 Co1 161.1(12) . .
C15 N11 C11 116.0(12) . .
C15 N11 Fe1 116.7(10) . .
C11 N11 Fe1 127.2(9) . .
C16 N12 C20 118.0(12) . .
C16 N12 Fe1 116.8(11) . .
C20 N12 Fe1 125.0(10) . .
N1O O1 Co1 118.7(11) . .
N1 C1 Fe1 177.6(11) . .
N2 C2 Fe1 169.8(17) . 2_554
N3 C3 Fe1 179(2) . .
N4 C4 Fe1 175.1(13) . 2_554
C12 C11 N11 122.4(15) . .
C11 C12 C13 120.1(16) . .
C14 C13 C12 117.7(15) . .
C14 C13 C21 126.5(15) . .
C12 C13 C21 115.3(14) . .
C15 C14 C13 115.8(15) . .
C14 C15 N11 127.6(16) . .
C14 C15 C16 119.2(13) . .
N11 C15 C16 113.2(12) . .
N12 C16 C17 122.7(15) . .
N12 C16 C15 113.5(12) . .
C17 C16 C15 123.8(14) . .
C16 C17 C18 120.4(16) . .
C19 C18 C17 116.8(16) . .
C19 C18 C22 119.5(18) . .
C17 C18 C22 123.7(17) . .
C20 C19 C18 118.1(19) . .
C19 C20 N12 123.9(17) . .
C4O C3O C2O 121(4) . .
C4O C3O C6O 125(4) . .
C2O C3O C6O 114(3) . .
N1O C5O C4O 114(4) . .
C3O C2O C1O 123(4) . .
N1O C1O C2O 118(4) . .
C3O C4O C5O 120(4) . .
C6O C6O C3O 119(4) 5_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.069(11) 5
Co1 N1 2.069(11) .
Co1 N4 2.086(11) .
Co1 N4 2.086(11) 5
Co1 O1 2.120(9) .
Co1 O1 2.120(9) 5
Fe1 C1 1.888(13) .
Fe1 C4 1.910(11) 2_554
Fe1 C3 1.928(14) .
Fe1 N11 1.935(10) .
Fe1 C2 1.966(16) 2_554
Fe1 N12 1.997(11) .
N1 C1 1.163(16) .
N1O O1 1.25(2) .
N1O C5O 1.28(4) .
N1O C1O 1.38(4) .
N2 C2 1.108(19) .
N3 C3 1.10(2) .
N4 C4 1.113(15) .
N11 C15 1.372(16) .
N11 C11 1.371(19) .
N12 C16 1.313(18) .
N12 C20 1.38(2) .
C2 Fe1 1.966(16) 2_554
C4 Fe1 1.910(11) 2_554
C11 C12 1.30(2) .
C12 C13 1.49(2) .
C13 C14 1.39(2) .
C13 C21 1.54(2) .
C14 C15 1.34(2) .
C15 C16 1.45(2) .
C16 C17 1.37(2) .
C17 C18 1.44(3) .
C18 C19 1.41(3) .
C18 C22 1.50(2) .
C19 C20 1.37(2) .
C3O C4O 1.24(4) .
C3O C2O 1.24(4) .
C3O C6O 1.58(4) .
C5O C4O 1.48(5) .
C2O C1O 1.36(4) .
C6O C6O 1.46(6) 5_565
