#------------------------------------------------------------------------------
#$Date: 2019-11-25 12:03:19 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240818 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/03/4130355.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_4130355
loop_
_publ_author_name
'Liu, Jiang'
'Chen, Yan-Cong'
'Liu, Jun-Liang'
'Vieru, Veacheslav'
'Ungur, Liviu'
'Jia, Jian-Hua'
'Chibotaru, Liviu F.'
'Lan, Yanhua'
'Wernsdorfer, Wolfgang'
'Gao, Song'
'Chen, Xiao-Ming'
'Tong, Ming-Liang'
_publ_section_title
;
 A Stable Pentagonal Bipyramidal Dy(III) Single-Ion Magnet with a Record
 Magnetization Reversal Barrier over 1000 K.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5441
_journal_page_last               5450
_journal_paper_doi               10.1021/jacs.6b02638
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration R
_chemical_formula_sum            'C28 H28 Cl N4 O2 Y'
_chemical_formula_weight         576.90
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C 2 2 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                   8.6871(4)
_cell_length_b                   17.1521(6)
_cell_length_c                   17.0046(6)
_cell_measurement_reflns_used    1925
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      60.9670
_cell_measurement_theta_min      5.6800
_cell_volume                     2533.72(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2839
_diffrn_reflns_theta_full        60.99
_diffrn_reflns_theta_max         60.99
_diffrn_reflns_theta_min         5.16
_exptl_absorpt_coefficient_mu    4.480
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90306
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0305
_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)+(0.0392P)²+1.8784P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                1638
_reflns_number_total             1697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b02638_si_004.cif
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      C222(1)
_cod_database_code               4130355
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
Y1 Y 0.5000 0.00801(2) 0.2500 0.01982(16) Uani 1 2 d S
Cl1 Cl 0.5000 -0.14699(7) 0.2500 0.0383(3) Uani 1 2 d S
O1 O 0.5970(3) 0.03578(16) 0.13661(16) 0.0257(6) Uani 1 1 d .
N1 N 0.6615(4) 0.13123(18) 0.27697(19) 0.0221(8) Uani 1 1 d .
N2 N 0.7534(4) -0.0177(2) 0.3225(2) 0.0269(8) Uani 1 1 d .
C1 C 0.8275(6) -0.0866(3) 0.3272(3) 0.0352(11) Uani 1 1 d .
H1 H 0.7825 -0.1307 0.3023 0.042 Uiso 1 1 calc R
C2 C 0.9651(5) -0.0966(3) 0.3664(3) 0.0382(13) Uani 1 1 d .
H2 H 1.0141 -0.1461 0.3676 0.046 Uiso 1 1 calc R
C3 C 1.0301(5) -0.0336(3) 0.4037(3) 0.0338(13) Uani 1 1 d .
H3 H 1.1246 -0.0388 0.4313 0.041 Uiso 1 1 calc R
C4 C 0.9559(5) 0.0373(3) 0.4003(2) 0.0282(12) Uani 1 1 d .
H4 H 0.9989 0.0817 0.4256 0.034 Uiso 1 1 calc R
C5 C 0.8177(5) 0.0435(2) 0.3596(2) 0.0226(9) Uani 1 1 d .
C6 C 0.7327(5) 0.1199(3) 0.3552(3) 0.0237(10) Uani 1 1 d .
H6A H 0.6516 0.1210 0.3961 0.028 Uiso 1 1 calc R
H6B H 0.8051 0.1632 0.3658 0.028 Uiso 1 1 calc R
C7 C 0.5650(5) 0.2030(2) 0.2803(2) 0.0239(9) Uani 1 1 d .
H7A H 0.6314 0.2490 0.2711 0.029 Uiso 1 1 calc R
H7B H 0.5201 0.2079 0.3335 0.029 Uiso 1 1 calc R
C8 C 0.7900(5) 0.1405(3) 0.2187(3) 0.0264(9) Uani 1 1 d .
H8A H 0.8540 0.1853 0.2353 0.032 Uiso 1 1 calc R
H8B H 0.8556 0.0934 0.2214 0.032 Uiso 1 1 calc R
C9 C 0.7443(5) 0.1528(3) 0.1350(3) 0.0238(10) Uani 1 1 d .
C10 C 0.8006(5) 0.2164(3) 0.0929(3) 0.0301(10) Uani 1 1 d .
H10 H 0.8628 0.2541 0.1187 0.036 Uiso 1 1 calc R
C11 C 0.7668(6) 0.2252(3) 0.0140(3) 0.0371(12) Uani 1 1 d .
H11 H 0.8062 0.2687 -0.0141 0.045 Uiso 1 1 calc R
C12 C 0.6761(6) 0.1712(3) -0.0241(3) 0.0350(11) Uani 1 1 d .
H12 H 0.6526 0.1779 -0.0782 0.042 Uiso 1 1 calc R
C13 C 0.6189(5) 0.1073(3) 0.0161(2) 0.0286(10) Uani 1 1 d .
H13 H 0.5571 0.0703 -0.0109 0.034 Uiso 1 1 calc R
C14 C 0.6510(5) 0.0964(2) 0.0966(3) 0.0241(9) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 '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
O1 Y1 O1 154.49(15) . 3_655
O1 Y1 N2 86.76(11) . 3_655
O1 Y1 N2 97.61(11) 3_655 3_655
O1 Y1 N2 97.61(11) . .
O1 Y1 N2 86.76(11) 3_655 .
N2 Y1 N2 160.21(15) 3_655 .
O1 Y1 N1 76.43(10) . .
O1 Y1 N1 82.68(11) 3_655 .
N2 Y1 N1 133.97(11) 3_655 .
N2 Y1 N1 65.64(11) . .
O1 Y1 N1 82.68(11) . 3_655
O1 Y1 N1 76.43(10) 3_655 3_655
N2 Y1 N1 65.64(11) 3_655 3_655
N2 Y1 N1 133.97(11) . 3_655
N1 Y1 N1 69.85(15) . 3_655
O1 Y1 Cl1 102.76(7) . .
O1 Y1 Cl1 102.76(7) 3_655 .
N2 Y1 Cl1 80.10(8) 3_655 .
N2 Y1 Cl1 80.10(8) . .
N1 Y1 Cl1 145.07(7) . .
N1 Y1 Cl1 145.07(7) 3_655 .
C14 O1 Y1 140.3(2) . .
C6 N1 C7 108.1(3) . .
C6 N1 C8 107.2(3) . .
C7 N1 C8 110.8(3) . .
C6 N1 Y1 106.2(2) . .
C7 N1 Y1 112.2(2) . .
C8 N1 Y1 112.0(2) . .
C5 N2 C1 117.2(4) . .
C5 N2 Y1 116.7(3) . .
C1 N2 Y1 126.1(3) . .
N2 C1 C2 123.4(4) . .
N2 C1 H1 118.3 . .
C2 C1 H1 118.3 . .
C3 C2 C1 118.8(4) . .
C3 C2 H2 120.6 . .
C1 C2 H2 120.6 . .
C2 C3 C4 118.9(4) . .
C2 C3 H3 120.6 . .
C4 C3 H3 120.6 . .
C3 C4 C5 119.5(4) . .
C3 C4 H4 120.3 . .
C5 C4 H4 120.3 . .
N2 C5 C4 122.2(4) . .
N2 C5 C6 116.8(4) . .
C4 C5 C6 121.0(4) . .
N1 C6 C5 111.4(4) . .
N1 C6 H6A 109.4 . .
C5 C6 H6A 109.4 . .
N1 C6 H6B 109.4 . .
C5 C6 H6B 109.4 . .
H6A C6 H6B 108.0 . .
N1 C7 C7 113.0(3) . 3_655
N1 C7 H7A 109.0 . .
C7 C7 H7A 109.0 3_655 .
N1 C7 H7B 109.0 . .
C7 C7 H7B 109.0 3_655 .
H7A C7 H7B 107.8 . .
C9 C8 N1 116.5(4) . .
C9 C8 H8A 108.2 . .
N1 C8 H8A 108.2 . .
C9 C8 H8B 108.2 . .
N1 C8 H8B 108.2 . .
H8A C8 H8B 107.3 . .
C10 C9 C14 119.7(4) . .
C10 C9 C8 120.5(4) . .
C14 C9 C8 119.6(4) . .
C11 C10 C9 120.7(5) . .
C11 C10 H10 119.7 . .
C9 C10 H10 119.7 . .
C12 C11 C10 120.3(4) . .
C12 C11 H11 119.9 . .
C10 C11 H11 119.9 . .
C11 C12 C13 120.3(4) . .
C11 C12 H12 119.8 . .
C13 C12 H12 119.8 . .
C12 C13 C14 121.0(4) . .
C12 C13 H13 119.5 . .
C14 C13 H13 119.5 . .
O1 C14 C13 122.1(4) . .
O1 C14 C9 119.9(4) . .
C13 C14 C9 118.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Y1 O1 2.158(3) .
Y1 O1 2.158(3) 3_655
Y1 N2 2.561(3) 3_655
Y1 N2 2.561(3) .
Y1 N1 2.578(3) .
Y1 N1 2.578(3) 3_655
Y1 Cl1 2.6586(12) .
O1 C14 1.328(5) .
N1 C6 1.480(6) .
N1 C7 1.490(5) .
N1 C8 1.501(5) .
N2 C5 1.345(5) .
N2 C1 1.349(6) .
C1 C2 1.380(7) .
C1 H1 0.9500 .
C2 C3 1.374(7) .
C2 H2 0.9500 .
C3 C4 1.378(7) .
C3 H3 0.9500 .
C4 C5 1.390(6) .
C4 H4 0.9500 .
C5 C6 1.506(7) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C7 1.528(8) 3_655
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.492(7) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.394(7) .
C9 C14 1.421(7) .
C10 C11 1.382(7) .
C10 H10 0.9500 .
C11 C12 1.377(7) .
C11 H11 0.9500 .
C12 C13 1.384(6) .
C12 H12 0.9500 .
C13 C14 1.408(6) .
C13 H13 0.9500 .
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
O1 Y1 O1 C14 10.7(4) 3_655 .
N2 Y1 O1 C14 111.6(4) 3_655 .
N2 Y1 O1 C14 -87.8(4) . .
N1 Y1 O1 C14 -25.2(4) . .
N1 Y1 O1 C14 45.7(4) 3_655 .
Cl1 Y1 O1 C14 -169.3(4) . .
O1 Y1 N1 C6 -141.9(3) . .
O1 Y1 N1 C6 52.8(3) 3_655 .
N2 Y1 N1 C6 146.4(2) 3_655 .
N2 Y1 N1 C6 -36.9(2) . .
N1 Y1 N1 C6 131.0(3) 3_655 .
Cl1 Y1 N1 C6 -49.0(3) . .
O1 Y1 N1 C7 100.2(3) . .
O1 Y1 N1 C7 -65.1(3) 3_655 .
N2 Y1 N1 C7 28.5(3) 3_655 .
N2 Y1 N1 C7 -154.8(3) . .
N1 Y1 N1 C7 13.13(19) 3_655 .
Cl1 Y1 N1 C7 -166.87(19) . .
O1 Y1 N1 C8 -25.2(2) . .
O1 Y1 N1 C8 169.6(3) 3_655 .
N2 Y1 N1 C8 -96.9(3) 3_655 .
N2 Y1 N1 C8 79.8(3) . .
N1 Y1 N1 C8 -112.2(3) 3_655 .
Cl1 Y1 N1 C8 67.8(3) . .
O1 Y1 N2 C5 91.6(3) . .
O1 Y1 N2 C5 -63.1(3) 3_655 .
N2 Y1 N2 C5 -166.7(3) 3_655 .
N1 Y1 N2 C5 20.3(3) . .
N1 Y1 N2 C5 4.5(4) 3_655 .
Cl1 Y1 N2 C5 -166.7(3) . .
O1 Y1 N2 C1 -88.8(4) . .
O1 Y1 N2 C1 116.5(4) 3_655 .
N2 Y1 N2 C1 12.9(4) 3_655 .
N1 Y1 N2 C1 -160.1(4) . .
N1 Y1 N2 C1 -175.9(3) 3_655 .
Cl1 Y1 N2 C1 12.9(4) . .
C5 N2 C1 C2 -1.3(7) . .
Y1 N2 C1 C2 179.1(4) . .
N2 C1 C2 C3 0.9(8) . .
C1 C2 C3 C4 -0.3(7) . .
C2 C3 C4 C5 0.1(6) . .
C1 N2 C5 C4 1.1(6) . .
Y1 N2 C5 C4 -179.3(3) . .
C1 N2 C5 C6 -178.9(4) . .
Y1 N2 C5 C6 0.7(5) . .
C3 C4 C5 N2 -0.5(6) . .
C3 C4 C5 C6 179.5(4) . .
C7 N1 C6 C5 173.5(3) . .
C8 N1 C6 C5 -67.0(4) . .
Y1 N1 C6 C5 52.9(4) . .
N2 C5 C6 N1 -37.8(5) . .
C4 C5 C6 N1 142.2(4) . .
C6 N1 C7 C7 -155.0(4) . 3_655
C8 N1 C7 C7 87.8(4) . 3_655
Y1 N1 C7 C7 -38.2(5) . 3_655
C6 N1 C8 C9 180.0(4) . .
C7 N1 C8 C9 -62.3(5) . .
Y1 N1 C8 C9 63.8(4) . .
N1 C8 C9 C10 126.3(4) . .
N1 C8 C9 C14 -57.9(6) . .
C14 C9 C10 C11 -0.1(7) . .
C8 C9 C10 C11 175.7(4) . .
C9 C10 C11 C12 0.3(7) . .
C10 C11 C12 C13 -0.5(7) . .
C11 C12 C13 C14 0.4(7) . .
Y1 O1 C14 C13 -139.4(4) . .
Y1 O1 C14 C9 40.5(6) . .
C12 C13 C14 O1 179.7(4) . .
C12 C13 C14 C9 -0.2(6) . .
C10 C9 C14 O1 -179.9(4) . .
C8 C9 C14 O1 4.3(6) . .
C10 C9 C14 C13 0.0(6) . .
C8 C9 C14 C13 -175.8(4) . .
