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
Ding, You-Song; Han, Tian; Hu, Yue-Qiao; Xu, Minwei; Yang, Sen; Zheng, Yan-Zhen; Inorganic Chemistry Frontiers 3 (2016) 798–; doi:10.1039/C5QI00308C

data_4349111
_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            'C20 H39 Cl3 Dy N O21'
_chemical_formula_weight         898.37
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-12-10 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.1940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   19.7259(6)
_cell_length_b                   17.2456(6)
_cell_length_c                   29.0850(9)
_cell_measurement_reflns_used    0.85
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      1.39
_cell_volume                     9452.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            79358
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    2.716
_exptl_absorpt_correction_T_max  0.6237
_exptl_absorpt_correction_T_min  0.5298
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5412
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.099
_refine_diff_density_min         -1.607
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1246
_refine_ls_number_reflns         21837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+31.9726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                18394
_reflns_number_total             21837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5qi00308c2.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C60 H117 Cl9 Dy3 N3 O63'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     2695.12
_cod_database_code               4349111