#------------------------------------------------------------------------------
#$Date: 2019-11-23 14:17:34 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233582 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/91/4349107.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_4349107
loop_
_publ_author_name
'Ding, You-Song'
'Han, Tian'
'Hu, Yue-Qiao'
'Xu, Minwei'
'Yang, Sen'
'Zheng, Yan-Zhen'
_publ_section_title
;
 Syntheses, structures and magnetic properties of a series of mono- and
 di-nuclear dysprosium(iii)-crown-ether complexes: effects of a weak
 ligand-field and flexible cyclic coordination modes
;
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              798
_journal_paper_doi               10.1039/C5QI00308C
_journal_volume                  3
_journal_year                    2016
_chemical_formula_sum            'C12 H24 Cl Dy N2 O16'
_chemical_formula_weight         650.28
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc141fsd
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-02-29 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.3304(18)
_cell_length_b                   10.8059(8)
_cell_length_c                   8.3756(6)
_cell_measurement_reflns_used    0.85
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      1.67
_cell_volume                     2202.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0109
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16108
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    3.595
_exptl_absorpt_correction_T_max  0.6219
_exptl_absorpt_correction_T_min  0.5639
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.918
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0333
_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)+(0.0289P)²+9.0094P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                2167
_reflns_number_total             2289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5qi00308c2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4349107
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Dy1 Dy 0.131354(11) 0.2500 0.91941(3) 0.03019(11) Uani 1 2 d S
Cl1 Cl 0.38380(10) 0.2500 0.9442(3) 0.0714(6) Uani 1 2 d S
N1 N 0.2122(2) 0.2500 0.6743(7) 0.0490(15) Uani 1 2 d S
N2 N 0.0444(2) 0.2500 1.1496(6) 0.0368(12) Uani 1 2 d S
C1 C 0.2386(3) 0.1352(9) 1.1345(12) 0.104(3) Uani 1 1 d .
H1A H 0.2632 0.0977 1.0536 0.125 Uiso 1 1 calc R
H1B H 0.2609 0.1525 1.2308 0.125 Uiso 1 1 calc R
C2 C 0.1991(5) 0.0536(9) 1.1722(16) 0.170(6) Uani 1 1 d .
H2A H 0.1834 0.0751 1.2778 0.204 Uiso 1 1 calc R
H2B H 0.2153 -0.0303 1.1800 0.204 Uiso 1 1 calc R
C3 C 0.1348(3) -0.0613(6) 1.0196(12) 0.097(3) Uani 1 1 d .
H3A H 0.1632 -0.1112 0.9645 0.117 Uiso 1 1 calc R
H3B H 0.1250 -0.1046 1.1197 0.117 Uiso 1 1 calc R
C4 C 0.0892(4) -0.0543(6) 0.9242(10) 0.089(2) Uani 1 1 d .
H4A H 0.0893 -0.1257 0.8502 0.107 Uiso 1 1 calc R
H4B H 0.0560 -0.0612 0.9922 0.107 Uiso 1 1 calc R
C5 C 0.0490(4) 0.0528(8) 0.7047(9) 0.103(3) Uani 1 1 d .
H5A H 0.0473 -0.0310 0.6573 0.124 Uiso 1 1 calc R
H5B H 0.0116 0.0752 0.7416 0.124 Uiso 1 1 calc R
C6 C 0.0664(3) 0.1372(7) 0.5901(8) 0.083(2) Uani 1 1 d .
H6A H 0.0357 0.1547 0.5157 0.099 Uiso 1 1 calc R
H6B H 0.0969 0.1004 0.5276 0.099 Uiso 1 1 calc R
O1 O 0.2173(2) 0.2500 1.0731(7) 0.0639(16) Uani 1 2 d S
O2 O 0.1568(2) 0.0531(4) 1.0572(6) 0.0908(17) Uani 1 1 d .
O3 O 0.0858(2) 0.0524(4) 0.8368(6) 0.0893(17) Uani 1 1 d .
O4 O 0.0845(2) 0.2500 0.6604(6) 0.0534(13) Uani 1 2 d S
O5 O 0.19518(14) 0.1506(3) 0.7365(5) 0.0547(9) Uani 1 1 d .
O6 O 0.2435(3) 0.2500 0.5605(8) 0.082(2) Uani 1 2 d S
O7 O 0.0928(2) 0.2500 1.1858(7) 0.091(3) Uani 1 2 d S
O8 O 0.0367(2) 0.2500 1.0074(7) 0.139(5) Uani 1 2 d S
O9 O 0.0072(2) 0.2500 1.2460(6) 0.0567(14) Uani 1 2 d S
O10 O 0.3356(3) 0.2500 0.8601(10) 0.112(3) Uani 1 2 d S
O11 O 0.4160(4) 0.1514(10) 0.9011(11) 0.206(5) Uani 1 1 d .
O12 O 0.3751(4) 0.2500 1.1101(10) 0.133(4) Uani 1 2 d S
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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
O8 Dy1 O7 49.47(19) . .
O8 Dy1 O5 143.17(13) . .
O7 Dy1 O5 145.92(12) . .
O8 Dy1 O5 143.17(13) . 7_565
O7 Dy1 O5 145.92(13) . 7_565
O5 Dy1 O5 52.41(17) . 7_565
O8 Dy1 O4 80.0(2) . .
O7 Dy1 O4 129.51(19) . .
O5 Dy1 O4 74.88(16) . .
O5 Dy1 O4 74.88(16) 7_565 .
O8 Dy1 O1 130.6(2) . .
O7 Dy1 O1 81.2(2) . .
O5 Dy1 O1 77.68(16) . .
O5 Dy1 O1 77.68(16) 7_565 .
O4 Dy1 O1 149.3(2) . .
O8 Dy1 O2 95.48(16) . 7_565
O7 Dy1 O2 70.75(15) . 7_565
O5 Dy1 O2 120.57(17) . 7_565
O5 Dy1 O2 75.90(17) 7_565 7_565
O4 Dy1 O2 121.61(10) . 7_565
O1 Dy1 O2 63.04(12) . 7_565
O8 Dy1 O2 95.49(17) . .
O7 Dy1 O2 70.75(15) . .
O5 Dy1 O2 75.90(17) . .
O5 Dy1 O2 120.56(17) 7_565 .
O4 Dy1 O2 121.61(10) . .
O1 Dy1 O2 63.04(12) . .
O2 Dy1 O2 116.8(2) 7_565 .
O8 Dy1 O3 70.26(15) . .
O7 Dy1 O3 94.78(15) . .
O5 Dy1 O3 74.47(17) . .
O5 Dy1 O3 119.04(16) 7_565 .
O4 Dy1 O3 63.21(10) . .
O1 Dy1 O3 121.48(10) . .
O2 Dy1 O3 164.5(2) 7_565 .
O2 Dy1 O3 60.75(14) . .
O8 Dy1 O3 70.26(15) . 7_565
O7 Dy1 O3 94.78(15) . 7_565
O5 Dy1 O3 119.04(16) . 7_565
O5 Dy1 O3 74.47(17) 7_565 7_565
O4 Dy1 O3 63.21(10) . 7_565
O1 Dy1 O3 121.48(10) . 7_565
O2 Dy1 O3 60.74(14) 7_565 7_565
O2 Dy1 O3 164.5(2) . 7_565
O3 Dy1 O3 117.0(2) . 7_565
O8 Dy1 N1 151.5(2) . .
O7 Dy1 N1 159.01(19) . .
O5 Dy1 N1 26.25(9) . .
O5 Dy1 N1 26.25(9) 7_565 .
O4 Dy1 N1 71.48(19) . .
O1 Dy1 N1 77.86(19) . .
O2 Dy1 N1 99.31(16) 7_565 .
O2 Dy1 N1 99.31(16) . .
O3 Dy1 N1 96.14(16) . .
O3 Dy1 N1 96.14(16) 7_565 .
O8 Dy1 N2 24.59(18) . .
O7 Dy1 N2 24.88(17) . .
O5 Dy1 N2 153.70(9) . .
O5 Dy1 N2 153.70(9) 7_565 .
O4 Dy1 N2 104.63(18) . .
O1 Dy1 N2 106.03(19) . .
O2 Dy1 N2 82.67(16) 7_565 .
O2 Dy1 N2 82.67(16) . .
O3 Dy1 N2 81.88(15) . .
O3 Dy1 N2 81.88(15) 7_565 .
N1 Dy1 N2 176.11(17) . .
O10 Cl1 O11 110.7(5) . 7_565
O10 Cl1 O11 110.7(5) . .
O11 Cl1 O11 102.0(10) 7_565 .
O10 Cl1 O12 112.3(6) . .
O11 Cl1 O12 110.3(5) 7_565 .
O11 Cl1 O12 110.3(5) . .
O6 N1 O5 121.8(3) . .
O6 N1 O5 121.8(3) . 7_565
O5 N1 O5 116.4(5) . 7_565
O6 N1 Dy1 174.9(6) . .
O5 N1 Dy1 58.4(3) . .
O5 N1 Dy1 58.4(3) 7_565 .
O8 N2 O9 122.8(6) . .
O8 N2 O7 113.3(6) . .
O9 N2 O7 123.9(6) . .
O8 N2 Dy1 56.6(4) . .
O9 N2 Dy1 179.4(4) . .
O7 N2 Dy1 56.7(3) . .
C2 C1 O1 113.0(6) . .
C1 C2 O2 111.4(9) . .
C4 C3 O2 113.4(6) . .
O3 C4 C3 114.0(6) . .
C6 C5 O3 110.3(6) . .
C5 C6 O4 111.7(6) . .
C1 O1 C1 119.0(9) . 7_565
C1 O1 Dy1 119.6(4) . .
C1 O1 Dy1 119.6(4) 7_565 .
C3 O2 C2 116.2(6) . .
C3 O2 Dy1 124.0(4) . .
C2 O2 Dy1 119.6(5) . .
C4 O3 C5 117.2(5) . .
C4 O3 Dy1 122.9(4) . .
C5 O3 Dy1 119.4(4) . .
C6 O4 C6 117.7(7) 7_565 .
C6 O4 Dy1 120.7(3) 7_565 .
C6 O4 Dy1 120.7(3) . .
N1 O5 Dy1 95.4(3) . .
N2 O7 Dy1 98.4(4) . .
N2 O8 Dy1 98.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O8 2.419(6) .
Dy1 O7 2.420(6) .
Dy1 O5 2.431(3) .
Dy1 O5 2.431(3) 7_565
Dy1 O4 2.450(5) .
Dy1 O1 2.455(5) .
Dy1 O2 2.499(4) 7_565
Dy1 O2 2.499(4) .
Dy1 O3 2.503(4) .
Dy1 O3 2.503(4) 7_565
Dy1 N1 2.843(6) .
Dy1 N2 2.863(5) .
Cl1 O10 1.368(8) .
Cl1 O11 1.371(8) 7_565
Cl1 O11 1.371(8) .
Cl1 O12 1.405(9) .
N1 O6 1.221(8) .
N1 O5 1.263(5) .
N1 O5 1.263(5) 7_565
N2 O8 1.206(8) .
N2 O9 1.212(7) .
N2 O7 1.217(7) .
C1 C2 1.342(12) .
C1 O1 1.440(8) .
C2 O2 1.409(9) .
C3 C4 1.370(10) .
C3 O2 1.383(8) .
C4 O3 1.369(7) .
C5 C6 1.390(10) .
C5 O3 1.423(8) .
C6 O4 1.424(7) .
O1 C1 1.440(8) 7_565
O4 C6 1.424(7) 7_565
