Fine-tuning the type of equatorial donor atom in pentagonal bipyramidal Dy(III) complexes to enhance single-molecule magnet properties
Wu, Haipeng; Li, Min; Yin, Bing; Xia, Zhengqiang; Ke, Hongshan; Wei, Qing; Xie, Gang; Chen, Sanping; Gao, Sheng-li; Dalton Transactions  (2019) –; doi:10.1039/C9DT03292D

data_7701289
_publ_section_title
;
 Fine-tuning the type of equatorial donor atom in pentagonal bipyramidal
 Dy(III) complexes to enhance single-molecule magnet properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03292D
_journal_year                    2019
_chemical_formula_moiety         'C14 H18 Cl3 Dy N4'
_chemical_formula_sum            'C14 H18 Cl3 Dy N4'
_chemical_formula_weight         511.17
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-16 deposited with the CCDC.    2019-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.659(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8991(12)
_cell_length_b                   9.1987(9)
_cell_length_c                   16.9903(17)
_cell_measurement_reflns_used    4113
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.52
_cell_volume                     1859.6(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10044
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.035
_diffrn_reflns_theta_min         1.711
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.449
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5926
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0246P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3281
_reflns_number_total             3991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03292d2.cif
_cod_data_source_block           1
_cod_database_code               7701289
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.617
_shelx_estimated_absorpt_t_min   0.536
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), N3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C7(H7A,H7B), C8(H8A,H8B), C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C1(H1), C4(H4), C3(H3A), C2(H2A), C11(H11), C12(H12), C13(H13)
;
_shelx_res_checksum              74836
_olex2_submission_special_instructions 'No special instructions were received'