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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/4/11/86/4118648.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_4118648
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 H34 Co Fe2 N14 O2'
_chemical_formula_weight         957.42
_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                 112.35(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.324(3)
_cell_length_b                   14.1543(4)
_cell_length_c                   11.9424(4)
_cell_measurement_temperature    293(2)
_cell_volume                     4740.8(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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15862
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         5.16
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.934
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            braun
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       naddels
_exptl_crystal_F_000             1948
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.813
_refine_ls_shift/su_mean         0.543
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1386P)²+65.1580P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2308
_refine_ls_wR_factor_ref         0.2576
_reflns_number_gt                2861
_reflns_number_total             4116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307042z_si_001.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        4740.8(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4118648
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
O1W O -0.1181(5) 0.5174(9) -0.3667(13) 0.155(4) Uani 1 1 d .
O2W O 0.0000 0.2836(15) -0.2500 0.201(7) Uani 1 2 d S
C1O C -0.0421(7) 0.2315(12) 0.0771(16) 0.128(5) Uani 1 1 d .
H1O H -0.0702 0.2002 0.0680 0.153 Uiso 1 1 calc R
C5O C 0.0493(8) 0.2325(10) 0.1365(18) 0.132(6) Uani 1 1 d .
H5O H 0.0796 0.2063 0.1724 0.159 Uiso 1 1 calc R
C2O C -0.0422(8) 0.3302(14) 0.0551(18) 0.144(6) Uani 1 1 d .
H2O H -0.0709 0.3631 0.0322 0.173 Uiso 1 1 calc R
C4O C 0.0400(7) 0.3275(13) 0.0946(19) 0.148(6) Uani 1 1 d .
H4O H 0.0651 0.3592 0.0849 0.178 Uiso 1 1 calc R
C3O C -0.0017(8) 0.3785(13) 0.067(2) 0.140(6) Uani 1 1 d .
C6O C -0.0029(9) 0.4884(15) 0.058(2) 0.169(7) Uani 1 1 d .
Co1 Co 0.0000 0.0000 0.0000 0.0223(4) Uani 1 2 d S
Fe1 Fe -0.13490(4) 0.10254(9) -0.37656(10) 0.0280(4) Uani 1 1 d .
N1 N -0.0509(3) 0.0805(6) -0.1359(6) 0.0394(18) Uani 1 1 d .
N1O N 0.0030(4) 0.1797(13) 0.1144(12) 0.110(5) Uani 1 1 d .
N2 N -0.1462(3) -0.1140(7) -0.3668(9) 0.064(3) Uani 1 1 d .
N3 N -0.1198(3) 0.3154(8) -0.3978(12) 0.082(3) Uani 1 1 d .
N4 N 0.0561(3) 0.0660(5) -0.0288(6) 0.0382(17) Uani 1 1 d .
N11 N -0.1905(2) 0.1083(5) -0.5309(6) 0.0330(16) Uani 1 1 d .
N12 N -0.1858(2) 0.1239(5) -0.3126(6) 0.0344(17) Uani 1 1 d .
O1 O 0.0024(2) 0.0969(4) 0.1352(5) 0.0389(15) Uani 1 1 d .
C1 C -0.0828(3) 0.0930(6) -0.2246(7) 0.0319(19) Uani 1 1 d .
C2 C -0.1421(3) -0.0353(7) -0.3710(8) 0.038(2) Uani 1 1 d .
C3 C -0.1250(3) 0.2362(7) -0.3870(9) 0.043(2) Uani 1 1 d .
C4 C 0.0868(3) 0.0818(6) -0.0602(7) 0.0311(18) Uani 1 1 d .
C11 C -0.1898(3) 0.1029(7) -0.6417(8) 0.042(2) Uani 1 1 d .
H11 H -0.1606 0.1014 -0.6501 0.050 Uiso 1 1 calc R
C12 C -0.2316(3) 0.0995(7) -0.7453(8) 0.047(2) Uani 1 1 d .
H12 H -0.2299 0.0932 -0.8210 0.056 Uiso 1 1 calc R
C13 C -0.2754(3) 0.1056(7) -0.7357(8) 0.047(2) Uani 1 1 d .
C14 C -0.2756(3) 0.1117(7) -0.6200(8) 0.043(2) Uani 1 1 d .
H14 H -0.3045 0.1140 -0.6099 0.051 Uiso 1 1 calc R
C15 C -0.2335(3) 0.1145(6) -0.5199(8) 0.036(2) Uani 1 1 d .
C17 C -0.2693(3) 0.1380(7) -0.3633(9) 0.044(2) Uani 1 1 d .
H17 H -0.3000 0.1387 -0.4226 0.053 Uiso 1 1 calc R
C18 C -0.2625(3) 0.1505(7) -0.2420(9) 0.046(2) Uani 1 1 d .
C19 C -0.2174(4) 0.1476(8) -0.1606(10) 0.055(3) Uani 1 1 d .
H19 H -0.2119 0.1552 -0.0790 0.066 Uiso 1 1 calc R
C20 C -0.1787(3) 0.1337(7) -0.1937(8) 0.042(2) Uani 1 1 d .
H20 H -0.1480 0.1311 -0.1348 0.051 Uiso 1 1 calc R
C21 C -0.3216(4) 0.1026(10) -0.8448(11) 0.075(4) Uani 1 1 d .
H21A H -0.3479 0.1076 -0.8191 0.112 Uiso 1 1 calc R
H21B H -0.3237 0.0439 -0.8870 0.112 Uiso 1 1 calc R
H21C H -0.3225 0.1542 -0.8978 0.112 Uiso 1 1 calc R
C22 C -0.3042(4) 0.1619(10) -0.2045(12) 0.069(4) Uani 1 1 d .
H22A H -0.3332 0.1623 -0.2751 0.103 Uiso 1 1 calc R
H22B H -0.3012 0.2203 -0.1615 0.103 Uiso 1 1 calc R
H22C H -0.3048 0.1103 -0.1529 0.103 Uiso 1 1 calc R
C16 C -0.2303(3) 0.1246(6) -0.3955(8) 0.036(2) 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'
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
N1O C1O C2O 119.0(18) . .
C4O C5O N1O 110.8(17) . .
C3O C2O C1O 122.2(18) . .
C3O C4O C5O 128.3(18) . .
C2O C3O C4O 117.9(18) . .
C2O C3O C6O 119.7(18) . .
C4O C3O C6O 122.3(19) . .
C6O C6O C3O 106(2) 5_565 .
N4 Co1 N4 180.0(4) 5 .
N4 Co1 O1 87.6(3) 5 .
N4 Co1 O1 92.4(3) . .
N4 Co1 O1 92.4(3) 5 5
N4 Co1 O1 87.6(3) . 5
O1 Co1 O1 180.0(4) . 5
N4 Co1 N1 88.0(3) 5 .
N4 Co1 N1 92.0(3) . .
O1 Co1 N1 92.3(3) . .
O1 Co1 N1 87.7(3) 5 .
N4 Co1 N1 92.0(3) 5 5
N4 Co1 N1 88.0(3) . 5
O1 Co1 N1 87.7(3) . 5
O1 Co1 N1 92.3(3) 5 5
N1 Co1 N1 180.0(7) . 5
C1 Fe1 C4 83.3(3) . 2_554
C1 Fe1 C3 92.2(4) . .
C4 Fe1 C3 87.9(4) 2_554 .
C1 Fe1 C2 87.7(4) . .
C4 Fe1 C2 88.5(4) 2_554 .
C3 Fe1 C2 176.3(4) . .
C1 Fe1 N11 177.3(3) . .
C4 Fe1 N11 98.5(3) 2_554 .
C3 Fe1 N11 89.9(3) . .
C2 Fe1 N11 90.3(3) . .
C1 Fe1 N12 97.4(3) . .
C4 Fe1 N12 179.3(3) 2_554 .
C3 Fe1 N12 92.2(3) . .
C2 Fe1 N12 91.4(3) . .
N11 Fe1 N12 80.8(3) . .
C1 N1 Co1 156.0(7) . .
O1 N1O C1O 117.7(14) . .
O1 N1O C5O 122.0(13) . .
C1O N1O C5O 120.0(17) . .
C4 N4 Co1 162.8(7) . .
C11 N11 C15 118.4(7) . .
C11 N11 Fe1 126.5(6) . .
C15 N11 Fe1 115.0(6) . .
C16 N12 C20 119.2(7) . .
C16 N12 Fe1 115.4(6) . .
C20 N12 Fe1 125.4(6) . .
N1O O1 Co1 118.6(8) . .
N1 C1 Fe1 174.8(8) . .
N2 C2 Fe1 179.4(9) . .
N3 C3 Fe1 177.4(11) . .
N4 C4 Fe1 175.5(8) . 2_554
N11 C11 C12 122.1(9) . .
C13 C12 C11 120.2(9) . .
C12 C13 C14 117.1(8) . .
C12 C13 C21 122.3(10) . .
C14 C13 C21 120.6(10) . .
C15 C14 C13 120.9(9) . .
N11 C15 C14 121.2(8) . .
N11 C15 C16 114.1(7) . .
C14 C15 C16 124.7(8) . .
C16 C17 C18 120.0(9) . .
C19 C18 C17 117.0(8) . .
C19 C18 C22 121.9(10) . .
C17 C18 C22 121.0(9) . .
C18 C19 C20 122.5(10) . .
N12 C20 C19 119.8(9) . .
N12 C16 C17 121.4(8) . .
N12 C16 C15 114.4(7) . .
C17 C16 C15 124.1(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1O N1O 1.46(2) .
C1O C2O 1.42(2) .
C5O C4O 1.42(2) .
C5O N1O 1.52(2) .
C2O C3O 1.37(2) .
C4O C3O 1.38(2) .
C3O C6O 1.56(3) .
C6O C6O 1.50(4) 5_565
Co1 N4 2.082(7) 5
Co1 N4 2.082(7) .
Co1 O1 2.098(6) .
Co1 O1 2.098(6) 5
Co1 N1 2.100(7) .
Co1 N1 2.100(7) 5
Fe1 C1 1.905(8) .
Fe1 C4 1.904(8) 2_554
Fe1 C3 1.927(11) .
Fe1 C2 1.967(11) .
Fe1 N11 1.971(7) .
Fe1 N12 1.989(7) .
N1 C1 1.144(10) .
N1O O1 1.200(18) .
N2 C2 1.124(12) .
N3 C3 1.147(13) .
N4 C4 1.149(10) .
N11 C11 1.333(11) .
N11 C15 1.363(11) .
N12 C16 1.335(11) .
N12 C20 1.360(11) .
C4 Fe1 1.904(8) 2_554
C11 C12 1.395(13) .
C12 C13 1.378(14) .
C13 C14 1.387(14) .
C13 C21 1.508(14) .
C14 C15 1.377(12) .
C15 C16 1.458(13) .
C17 C16 1.390(12) .
C17 C18 1.394(14) .
C18 C19 1.346(14) .
C18 C22 1.500(12) .
C19 C20 1.386(13) .
