#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/69/4106907.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_4106907
loop_
_publ_author_name
'Titel Jurca'
'Ahmed Farghal'
'Po-Heng Lin'
'Ilia Korobkov'
'Muralee Murugesu'
'Darrin S. Richeson'
_publ_section_title
;
 Single-Molecule Magnet Behavior with a Single Metal Center Enhanced
 through Peripheral Ligand Modifications
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15814
_journal_page_last               15817
_journal_paper_doi               10.1021/ja204562m
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C47 H51 Co N5 O0.5 S2'
_chemical_formula_weight         816.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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            4
_cell_length_a                   16.2916(5)
_cell_length_b                   18.6440(6)
_cell_length_c                   15.7275(5)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.34
_cell_measurement_theta_min      2.54
_cell_volume                     4777.1(3)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.1278
_diffrn_reflns_av_sigmaI/netI    0.1191
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            66076
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.9857
_exptl_absorpt_correction_T_min  0.9225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       needle
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         6018
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1705
_refine_ls_R_factor_gt           0.0693
_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)+(0.0579P)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                3165
_reflns_number_total             6018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204562m_si_002.cif
_cod_data_source_block           dr011
_cod_original_formula_sum        'C47 H51 Co N5 O0.50 S2'
_cod_database_code               4106907
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, 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
Co1 Co 1.0000 0.90240(3) 0.09397(4) 0.0435(2) Uani 1 2 d S
S1 S 1.0000 0.71384(10) 0.28917(13) 0.1000(7) Uani 1 2 d S
S2 S 1.0000 0.88458(16) -0.20675(12) 0.1292(10) Uani 1 2 d S
N1 N 0.86931(18) 0.93264(15) 0.11279(17) 0.0418(8) Uani 1 1 d .
N2 N 1.0000 1.01192(18) 0.0992(3) 0.0375(9) Uani 1 2 d S
N3 N 1.0000 0.8148(3) 0.1615(3) 0.0629(14) Uani 1 2 d S
N4 N 1.0000 0.8979(3) -0.0311(3) 0.0601(14) Uani 1 2 d S
C1 C 0.8551(2) 0.99994(18) 0.1056(2) 0.0398(8) Uani 1 1 d .
C2 C 0.7746(2) 1.0357(2) 0.1148(2) 0.0467(10) Uani 1 1 d .
C3 C 0.7646(3) 1.0932(2) 0.1698(3) 0.0592(11) Uani 1 1 d .
H3A H 0.8088 1.1093 0.2019 0.071 Uiso 1 1 calc R
C4 C 0.6895(3) 1.1264(3) 0.1771(3) 0.0760(14) Uani 1 1 d .
H4A H 0.6828 1.1646 0.2145 0.091 Uiso 1 1 calc R
C5 C 0.6252(3) 1.1030(3) 0.1294(4) 0.0867(17) Uani 1 1 d .
H5A H 0.5747 1.1258 0.1344 0.104 Uiso 1 1 calc R
C6 C 0.6332(3) 1.0475(3) 0.0749(4) 0.0822(16) Uani 1 1 d .
H6A H 0.5887 1.0326 0.0425 0.099 Uiso 1 1 calc R
C7 C 0.7078(3) 1.0130(2) 0.0676(3) 0.0602(12) Uani 1 1 d .
H7A H 0.7133 0.9743 0.0308 0.072 Uiso 1 1 calc R
C8 C 0.9287(2) 1.04574(16) 0.0885(3) 0.0387(8) Uani 1 1 d .
C9 C 0.9274(2) 1.1171(2) 0.0658(2) 0.0486(11) Uani 1 1 d .
H9A H 0.8777 1.1411 0.0592 0.058 Uiso 1 1 calc R
C10 C 1.0000 1.1522(3) 0.0529(4) 0.0574(17) Uani 1 2 d S
H10A H 1.0000 1.1998 0.0355 0.069 Uiso 1 2 calc SR
C11 C 0.8056(3) 0.8839(2) 0.1406(2) 0.0472(10) Uani 1 1 d .
C12 C 0.7725(3) 0.83577(19) 0.0829(3) 0.0618(12) Uani 1 1 d .
C13 C 0.7127(4) 0.7890(2) 0.1127(4) 0.0944(19) Uani 1 1 d .
H13A H 0.6873 0.7575 0.0752 0.113 Uiso 1 1 calc R
C14 C 0.6903(4) 0.7889(3) 0.1977(5) 0.105(2) Uani 1 1 d .
H14A H 0.6502 0.7573 0.2169 0.126 Uiso 1 1 calc R
C15 C 0.7268(4) 0.8345(3) 0.2527(4) 0.0825(18) Uani 1 1 d .
H15A H 0.7124 0.8327 0.3098 0.099 Uiso 1 1 calc R
C16 C 0.7844(3) 0.8833(2) 0.2270(3) 0.0535(12) Uani 1 1 d .
C17 C 0.8000(3) 0.8319(2) -0.0104(3) 0.0727(14) Uani 1 1 d .
H17A H 0.8338 0.8743 -0.0221 0.087 Uiso 1 1 calc R
C18 C 0.7266(4) 0.8328(3) -0.0731(4) 0.112(2) Uani 1 1 d .
H18A H 0.7467 0.8307 -0.1304 0.169 Uiso 1 1 calc R
H18B H 0.6956 0.8761 -0.0652 0.169 Uiso 1 1 calc R
H18C H 0.6920 0.7921 -0.0624 0.169 Uiso 1 1 calc R
C19 C 0.8537(3) 0.7657(3) -0.0236(3) 0.0915(17) Uani 1 1 d .
H19A H 0.8995 0.7673 0.0148 0.137 Uiso 1 1 calc R
H19B H 0.8735 0.7648 -0.0811 0.137 Uiso 1 1 calc R
H19C H 0.8220 0.7232 -0.0129 0.137 Uiso 1 1 calc R
C20 C 0.8238(3) 0.9322(2) 0.2913(3) 0.0709(13) Uani 1 1 d .
H20A H 0.8564 0.9678 0.2603 0.085 Uiso 1 1 calc R
C21 C 0.7616(4) 0.9724(3) 0.3456(4) 0.135(3) Uani 1 1 d .
H21A H 0.7249 0.9988 0.3094 0.202 Uiso 1 1 calc R
H21B H 0.7898 1.0051 0.3827 0.202 Uiso 1 1 calc R
H21C H 0.7307 0.9388 0.3790 0.202 Uiso 1 1 calc R
C22 C 0.8802(6) 0.8923(4) 0.3488(4) 0.153(3) Uani 1 1 d .
H22A H 0.9204 0.8672 0.3156 0.229 Uiso 1 1 calc R
H22B H 0.8493 0.8585 0.3820 0.229 Uiso 1 1 calc R
H22C H 0.9074 0.9255 0.3861 0.229 Uiso 1 1 calc R
C23 C 1.0000 0.7730(3) 0.2149(4) 0.0597(17) Uani 1 2 d S
C24 C 1.0000 0.8933(3) -0.1030(4) 0.0609(17) Uani 1 2 d S
O1 O 0.0000 0.4655(7) 0.4043(7) 0.099(3) Uani 0.50 2 d SP
C25 C 0.0000 0.5081(12) 0.333(2) 0.130(7) Uani 0.50 2 d SP
H25A H 0.0486 0.5381 0.3300 0.156 Uiso 0.25 1 calc PR
H25B H -0.0486 0.5381 0.3300 0.156 Uiso 0.25 1 calc PR
C26 C 0.0000 0.453(2) 0.2647(13) 0.181(15) Uani 0.50 2 d SP
H26A H 0.0483 0.4582 0.2292 0.217 Uiso 0.25 1 calc PR
H26B H -0.0483 0.4582 0.2292 0.217 Uiso 0.25 1 calc PR
C27 C 0.0000 0.3825(17) 0.304(2) 0.158(13) Uani 0.50 2 d SP
H27A H -0.0486 0.3552 0.2894 0.189 Uiso 0.25 1 calc PR
H27B H 0.0486 0.3552 0.2894 0.189 Uiso 0.25 1 calc PR
C28 C 0.0000 0.3992(12) 0.3796(15) 0.119(7) Uani 0.50 2 d SP
H28A H 0.0477 0.3767 0.4050 0.142 Uiso 0.25 1 calc PR
H28B H -0.0477 0.3767 0.4050 0.142 Uiso 0.25 1 calc PR
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'
S S 0.1246 0.1234 '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'
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 Co1 N4 120.6(2) . .
N3 Co1 N2 144.6(2) . .
N4 Co1 N2 94.8(2) . .
N3 Co1 N1 98.05(8) . .
N4 Co1 N1 98.28(8) . .
N2 Co1 N1 74.99(8) . .
N3 Co1 N1 98.05(8) . 4_755
N4 Co1 N1 98.28(8) . 4_755
N2 Co1 N1 74.99(8) . 4_755
N1 Co1 N1 146.69(15) . 4_755
C1 N1 C11 120.8(3) . .
C1 N1 Co1 114.2(2) . .
C11 N1 Co1 124.6(2) . .
C8 N2 C8 121.3(4) 4_755 .
C8 N2 Co1 117.89(19) 4_755 .
C8 N2 Co1 117.89(19) . .
C23 N3 Co1 165.9(5) . .
C24 N4 Co1 178.2(5) . .
N1 C1 C2 126.4(3) . .
N1 C1 C8 115.5(3) . .
C2 C1 C8 118.1(3) . .
C7 C2 C3 118.6(4) . .
C7 C2 C1 120.5(4) . .
C3 C2 C1 120.9(4) . .
C4 C3 C2 120.3(4) . .
C5 C4 C3 119.6(5) . .
C6 C5 C4 121.4(5) . .
C5 C6 C7 119.7(5) . .
C2 C7 C6 120.4(4) . .
N2 C8 C9 120.2(3) . .
N2 C8 C1 113.9(3) . .
C9 C8 C1 125.8(3) . .
C10 C9 C8 119.1(4) . .
C9 C10 C9 120.0(5) . 4_755
C12 C11 C16 122.4(4) . .
C12 C11 N1 119.2(3) . .
C16 C11 N1 118.3(4) . .
C11 C12 C13 117.2(5) . .
C11 C12 C17 122.9(4) . .
C13 C12 C17 119.9(4) . .
C14 C13 C12 120.8(5) . .
C15 C14 C13 120.0(5) . .
C14 C15 C16 122.1(5) . .
C15 C16 C11 117.3(5) . .
C15 C16 C20 119.8(4) . .
C11 C16 C20 122.8(4) . .
C19 C17 C12 109.6(4) . .
C19 C17 C18 111.3(4) . .
C12 C17 C18 112.4(5) . .
C22 C20 C16 111.6(4) . .
C22 C20 C21 108.4(5) . .
C16 C20 C21 113.0(5) . .
N3 C23 S1 179.5(6) . .
N4 C24 S2 178.6(6) . .
C28 O1 C25 107.7(17) . .
O1 C25 C26 100.9(17) . .
C25 C26 C27 108.5(18) . .
C28 C27 C26 101(2) . .
C27 C28 O1 122(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N3 1.949(5) .
Co1 N4 1.968(5) .
Co1 N2 2.044(3) .
Co1 N1 2.222(3) .
Co1 N1 2.222(3) 4_755
S1 C23 1.606(7) .
S2 C24 1.640(6) .
N1 C1 1.281(4) .
N1 C11 1.448(5) .
N2 C8 1.332(4) 4_755
N2 C8 1.332(4) .
N3 C23 1.145(7) .
N4 C24 1.134(7) .
C1 C2 1.478(5) .
C1 C8 1.496(5) .
C2 C7 1.382(5) .
C2 C3 1.387(5) .
C3 C4 1.376(6) .
C4 C5 1.360(7) .
C5 C6 1.350(7) .
C6 C7 1.380(6) .
C8 C9 1.378(5) .
C9 C10 1.366(5) .
C10 C9 1.366(5) 4_755
C11 C12 1.385(6) .
C11 C16 1.402(5) .
C12 C13 1.389(6) .
C12 C17 1.536(7) .
C13 C14 1.386(8) .
C14 C15 1.351(9) .
C15 C16 1.368(7) .
C16 C20 1.505(6) .
C17 C19 1.527(7) .
C17 C18 1.550(7) .
C20 C22 1.489(8) .
C20 C21 1.523(7) .
O1 C28 1.30(2) .
O1 C25 1.38(2) .
C25 C26 1.49(3) .
C26 C27 1.45(3) .
C27 C28 1.22(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N3 Co1 N1 C1 154.0(3) . .
N4 Co1 N1 C1 -83.3(3) . .
N2 Co1 N1 C1 9.5(3) . .
N1 Co1 N1 C1 35.8(4) 4_755 .
N3 Co1 N1 C11 -19.0(3) . .
N4 Co1 N1 C11 103.7(3) . .
N2 Co1 N1 C11 -163.5(3) . .
N1 Co1 N1 C11 -137.2(3) 4_755 .
N3 Co1 N2 C8 99.5(4) . 4_755
N4 Co1 N2 C8 -80.5(4) . 4_755
N1 Co1 N2 C8 -177.8(4) . 4_755
N1 Co1 N2 C8 16.8(4) 4_755 4_755
N3 Co1 N2 C8 -99.5(4) . .
N4 Co1 N2 C8 80.5(4) . .
N1 Co1 N2 C8 -16.8(4) . .
N1 Co1 N2 C8 177.8(4) 4_755 .
N4 Co1 N3 C23 180.000(7) . .
N2 Co1 N3 C23 0.000(8) . .
N1 Co1 N3 C23 -75.37(8) . .
N1 Co1 N3 C23 75.38(8) 4_755 .
N3 Co1 N4 C24 0.00(6) . .
N2 Co1 N4 C24 180.00(6) . .
N1 Co1 N4 C24 -104.50(10) . .
N1 Co1 N4 C24 104.50(10) 4_755 .
C11 N1 C1 C2 -6.7(6) . .
Co1 N1 C1 C2 -180.0(3) . .
C11 N1 C1 C8 171.6(3) . .
Co1 N1 C1 C8 -1.7(4) . .
N1 C1 C2 C7 -53.6(6) . .
C8 C1 C2 C7 128.2(4) . .
N1 C1 C2 C3 127.2(4) . .
C8 C1 C2 C3 -51.0(5) . .
C7 C2 C3 C4 0.2(6) . .
C1 C2 C3 C4 179.4(4) . .
C2 C3 C4 C5 -0.6(7) . .
C3 C4 C5 C6 0.3(8) . .
C4 C5 C6 C7 0.5(8) . .
C3 C2 C7 C6 0.6(6) . .
C1 C2 C7 C6 -178.6(4) . .
C5 C6 C7 C2 -1.0(7) . .
C8 N2 C8 C9 0.0(8) 4_755 .
Co1 N2 C8 C9 -160.3(3) . .
C8 N2 C8 C1 -178.4(3) 4_755 .
Co1 N2 C8 C1 21.3(5) . .
N1 C1 C8 N2 -12.1(6) . .
C2 C1 C8 N2 166.3(4) . .
N1 C1 C8 C9 169.6(4) . .
C2 C1 C8 C9 -12.0(6) . .
N2 C8 C9 C10 1.2(7) . .
C1 C8 C9 C10 179.4(4) . .
C8 C9 C10 C9 -2.4(8) . 4_755
C1 N1 C11 C12 110.0(4) . .
Co1 N1 C11 C12 -77.5(4) . .
C1 N1 C11 C16 -75.1(5) . .
Co1 N1 C11 C16 97.4(4) . .
C16 C11 C12 C13 4.1(6) . .
N1 C11 C12 C13 178.7(4) . .
C16 C11 C12 C17 -175.1(4) . .
N1 C11 C12 C17 -0.4(6) . .
C11 C12 C13 C14 -2.9(7) . .
C17 C12 C13 C14 176.3(5) . .
C12 C13 C14 C15 0.0(9) . .
C13 C14 C15 C16 2.0(9) . .
C14 C15 C16 C11 -0.9(8) . .
C14 C15 C16 C20 -179.3(5) . .
C12 C11 C16 C15 -2.3(6) . .
N1 C11 C16 C15 -177.0(4) . .
C12 C11 C16 C20 176.1(4) . .
N1 C11 C16 C20 1.4(6) . .
C11 C12 C17 C19 105.2(5) . .
C13 C12 C17 C19 -73.9(6) . .
C11 C12 C17 C18 -130.4(5) . .
C13 C12 C17 C18 50.5(6) . .
C15 C16 C20 C22 70.3(6) . .
C11 C16 C20 C22 -108.0(6) . .
C15 C16 C20 C21 -52.2(6) . .
C11 C16 C20 C21 129.4(5) . .
Co1 N3 C23 S1 -180.0(3) . .
Co1 N4 C24 S2 0.00(13) . .
C28 O1 C25 C26 0.000(5) . .
O1 C25 C26 C27 0.000(6) . .
C25 C26 C27 C28 0.000(7) . .
C26 C27 C28 O1 0.000(5) . .
C25 O1 C28 C27 0.000(5) . .
