#------------------------------------------------------------------------------
#$Date: 2021-06-05 22:19:32 +0300 (Sat, 05 Jun 2021) $
#$Revision: 266131 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/05/7060549.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_7060549
loop_
_publ_author_name
'Zhang, Chunyang'
'Cheng, Zhijie'
'Tan, Pengfei'
'Lv, Wei'
'Cui, Huihui'
'Chen, Lei'
'Cai, Xingwei'
'Zhao, Yuyuan'
'Yuan, Aihua'
_publ_section_title
;
 Tuning the ligand field in seven-coordinate Dy(iii) complexes to perturb
 single-ion magnet behavior
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8591
_journal_page_last               8596
_journal_paper_doi               10.1039/D1NJ00734C
_journal_volume                  45
_journal_year                    2021
_chemical_formula_sum            'C18 H18 Cl3 Dy N4'
_chemical_formula_weight         559.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-02-10 deposited with the CCDC.	2021-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.2820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.65720(10)
_cell_length_b                   16.2902(2)
_cell_length_c                   14.7873(2)
_cell_measurement_reflns_used    12244
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.477
_cell_measurement_theta_min      2.428
_cell_volume                     2020.96(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21846
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         2.731
_exptl_absorpt_coefficient_mu    4.103
_exptl_absorpt_correction_T_max  0.5968
_exptl_absorpt_correction_T_min  0.4803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0247P)²+0.4200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.0471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4080
_reflns_number_total             4625
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj00734c2.cif
_cod_data_source_block           '[Dy(TPA)Cl3]'
_cod_depositor_comments
'Adding full bibliography for 7060549--7060550.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7060549
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.480
_shelx_estimated_absorpt_t_max   0.597
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.72222(2) 0.14831(2) 0.75688(2) 0.02515(4) Uani 1 1 d . . . . .
N1 N 0.5151(2) 0.24011(11) 0.80486(12) 0.0244(4) Uani 1 1 d . . . . .
N2 N 0.4586(2) 0.16073(12) 0.63561(14) 0.0327(5) Uani 1 1 d . . . . .
N3 N 0.7983(2) 0.29688(13) 0.78029(15) 0.0344(5) Uani 1 1 d . . . . .
N4 N 0.6718(3) 0.11844(14) 0.91595(14) 0.0372(5) Uani 1 1 d . . . . .
Cl1 Cl 0.64187(8) -0.00716(4) 0.74026(5) 0.04401(16) Uani 1 1 d . . . . .
Cl2 Cl 1.01911(8) 0.13019(5) 0.84839(6) 0.0571(2) Uani 1 1 d . . . . .
Cl3 Cl 0.81806(10) 0.15393(6) 0.60326(5) 0.0640(3) Uani 1 1 d . . . . .
C1 C 0.4046(3) 0.27731(15) 0.72235(16) 0.0325(5) Uani 1 1 d . . . . .
H1A H 0.457055 0.323276 0.700726 0.039 Uiso 1 1 calc R U . . .
H1B H 0.311711 0.298287 0.740448 0.039 Uiso 1 1 calc R U . . .
C2 C 0.3518(3) 0.21738(15) 0.64415(15) 0.0297(5) Uani 1 1 d . . . . .
C3 C 0.2051(3) 0.22362(19) 0.58174(18) 0.0474(7) Uani 1 1 d . . . . .
H3 H 0.132330 0.263208 0.589887 0.057 Uiso 1 1 calc R U . . .
C4 C 0.1677(3) 0.1705(2) 0.5072(2) 0.0549(8) Uani 1 1 d . . . . .
H4 H 0.069583 0.174180 0.464036 0.066 Uiso 1 1 calc R U . . .
C5 C 0.2764(3) 0.1120(2) 0.49711(18) 0.0475(7) Uani 1 1 d . . . . .
H5 H 0.253319 0.075237 0.447437 0.057 Uiso 1 1 calc R U . . .
C6 C 0.4200(3) 0.10903(18) 0.56212(17) 0.0412(6) Uani 1 1 d . . . . .
H6 H 0.494050 0.069651 0.555273 0.049 Uiso 1 1 calc R U . . .
C7 C 0.4235(3) 0.18885(17) 0.85538(16) 0.0342(5) Uani 1 1 d . . . . .
H7A H 0.356176 0.151286 0.812000 0.041 Uiso 1 1 calc R U . . .
H7B H 0.355053 0.223650 0.881928 0.041 Uiso 1 1 calc R U . . .
C8 C 0.5323(3) 0.14085(14) 0.93180(17) 0.0328(6) Uani 1 1 d . . . . .
C9 C 0.4885(4) 0.11950(18) 1.01238(19) 0.0475(7) Uani 1 1 d . . . . .
H9 H 0.391336 0.136773 1.021958 0.057 Uiso 1 1 calc R U . . .
C10 C 0.5902(5) 0.07237(18) 1.07827(19) 0.0562(9) Uani 1 1 d . . . . .
H10 H 0.562901 0.057187 1.132928 0.067 Uiso 1 1 calc R U . . .
C11 C 0.7308(4) 0.04844(19) 1.06225(19) 0.0573(9) Uani 1 1 d . . . . .
H11 H 0.800754 0.016044 1.105624 0.069 Uiso 1 1 calc R U . . .
C12 C 0.7696(4) 0.07235(18) 0.98139(18) 0.0512(8) Uani 1 1 d . . . . .
H12 H 0.867080 0.056058 0.971544 0.061 Uiso 1 1 calc R U . . .
C13 C 0.5961(3) 0.30705(15) 0.86661(16) 0.0319(5) Uani 1 1 d . . . . .
H13A H 0.640106 0.285294 0.928690 0.038 Uiso 1 1 calc R U . . .
H13B H 0.518635 0.348897 0.871185 0.038 Uiso 1 1 calc R U . . .
C14 C 0.7267(3) 0.34501(14) 0.83095(17) 0.0320(5) Uani 1 1 d . . . . .
C15 C 0.7754(4) 0.42530(17) 0.8525(2) 0.0481(7) Uani 1 1 d . . . . .
H15 H 0.722879 0.458121 0.886870 0.058 Uiso 1 1 calc R U . . .
C16 C 0.9019(4) 0.4557(2) 0.8225(2) 0.0557(8) Uani 1 1 d . . . . .
H16 H 0.936772 0.509256 0.836743 0.067 Uiso 1 1 calc R U . . .
C17 C 0.9759(4) 0.4067(2) 0.7716(2) 0.0558(8) Uani 1 1 d . . . . .
H17 H 1.061969 0.426039 0.750678 0.067 Uiso 1 1 calc R U . . .
C18 C 0.9211(3) 0.32844(19) 0.7519(2) 0.0489(7) Uani 1 1 d . . . . .
H18 H 0.971873 0.295337 0.716804 0.059 Uiso 1 1 calc R U . . .
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'
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
_geom_angle_publ_flag
N3 Dy1 N2 100.38(7) . . ?
N3 Dy1 N4 98.98(7) . . ?
N2 Dy1 N4 109.82(7) . . ?
N3 Dy1 N1 65.00(6) . . ?
N2 Dy1 N1 65.23(6) . . ?
N4 Dy1 N1 64.19(6) . . ?
N3 Dy1 Cl3 87.54(5) . . ?
N2 Dy1 Cl3 78.78(5) . . ?
N4 Dy1 Cl3 167.84(5) . . ?
N1 Dy1 Cl3 127.97(4) . . ?
N3 Dy1 Cl2 81.15(5) . . ?
N2 Dy1 Cl2 166.93(5) . . ?
N4 Dy1 Cl2 82.57(5) . . ?
N1 Dy1 Cl2 126.07(4) . . ?
Cl3 Dy1 Cl2 88.36(3) . . ?
N3 Dy1 Cl1 177.42(5) . . ?
N2 Dy1 Cl1 80.75(5) . . ?
N4 Dy1 Cl1 78.45(5) . . ?
N1 Dy1 Cl1 113.67(4) . . ?
Cl3 Dy1 Cl1 94.96(3) . . ?
Cl2 Dy1 Cl1 98.28(2) . . ?
C7 N1 C1 109.27(18) . . ?
C7 N1 C13 109.63(18) . . ?
C1 N1 C13 108.51(18) . . ?
C7 N1 Dy1 108.05(14) . . ?
C1 N1 Dy1 111.35(13) . . ?
C13 N1 Dy1 110.02(13) . . ?
C2 N2 C6 117.9(2) . . ?
C2 N2 Dy1 120.76(15) . . ?
C6 N2 Dy1 121.32(17) . . ?
C14 N3 C18 117.7(2) . . ?
C14 N3 Dy1 120.04(16) . . ?
C18 N3 Dy1 121.9(2) . . ?
C8 N4 C12 117.5(2) . . ?
C8 N4 Dy1 118.60(16) . . ?
C12 N4 Dy1 123.40(19) . . ?
N1 C1 C2 112.43(19) . . ?
N2 C2 C3 122.3(2) . . ?
N2 C2 C1 115.98(19) . . ?
C3 C2 C1 121.7(2) . . ?
C2 C3 C4 119.1(3) . . ?
C5 C4 C3 119.4(3) . . ?
C6 C5 C4 118.3(3) . . ?
N2 C6 C5 123.0(3) . . ?
N1 C7 C8 111.1(2) . . ?
N4 C8 C9 122.3(2) . . ?
N4 C8 C7 115.9(2) . . ?
C9 C8 C7 121.7(3) . . ?
C10 C9 C8 119.2(3) . . ?
C11 C10 C9 118.9(3) . . ?
C10 C11 C12 119.6(3) . . ?
N4 C12 C11 122.5(3) . . ?
N1 C13 C14 111.77(19) . . ?
N3 C14 C15 121.7(3) . . ?
N3 C14 C13 116.8(2) . . ?
C15 C14 C13 121.5(2) . . ?
C16 C15 C14 119.2(3) . . ?
C17 C16 C15 119.3(3) . . ?
C16 C17 C18 118.7(3) . . ?
N3 C18 C17 123.5(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 N3 2.510(2) . ?
Dy1 N2 2.539(2) . ?
Dy1 N4 2.543(2) . ?
Dy1 N1 2.5658(18) . ?
Dy1 Cl3 2.6052(7) . ?
Dy1 Cl2 2.6093(7) . ?
Dy1 Cl1 2.6218(7) . ?
N1 C7 1.475(3) . ?
N1 C1 1.482(3) . ?
N1 C13 1.483(3) . ?
N2 C2 1.334(3) . ?
N2 C6 1.350(3) . ?
N3 C14 1.337(3) . ?
N3 C18 1.339(3) . ?
N4 C8 1.336(3) . ?
N4 C12 1.346(3) . ?
C1 C2 1.496(3) . ?
C2 C3 1.377(3) . ?
C3 C4 1.376(4) . ?
C4 C5 1.374(4) . ?
C5 C6 1.372(3) . ?
C7 C8 1.500(3) . ?
C8 C9 1.381(4) . ?
C9 C10 1.375(4) . ?
C10 C11 1.353(5) . ?
C11 C12 1.375(4) . ?
C13 C14 1.495(4) . ?
C14 C15 1.387(3) . ?
C15 C16 1.372(4) . ?
C16 C17 1.361(5) . ?
C17 C18 1.366(4) . ?
