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_7701291
_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         'C26 H22 Br4 Cl Dy N6 O6'
_chemical_formula_sum            'C26 H22 Br4 Cl Dy N6 O6'
_chemical_formula_weight         1032.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                93.466(6)
_cell_angle_beta                 95.632(7)
_cell_angle_gamma                110.499(9)
_cell_formula_units_Z            2
_cell_length_a                   8.2337(8)
_cell_length_b                   11.3866(8)
_cell_length_c                   18.9912(14)
_cell_measurement_reflns_used    2833
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.1370
_cell_measurement_theta_min      4.5610
_cell_volume                     1651.1(3)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.1162
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11400
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.732
_diffrn_reflns_theta_min         4.167
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    18.939
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0706 before and 0.0372 after correction. The Ratio of minimum to maximum transmission is 0.7949. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_description       block
_exptl_crystal_F_000             982
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.925
_refine_diff_density_min         -1.624
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_gt           0.0930
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0974P)^2^+18.7156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2434
_refine_ls_wR_factor_ref         0.2682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4227
_reflns_number_total             6179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03292d2.cif
_cod_data_source_block           2
_cod_database_code               7701291
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.177
_shelx_estimated_absorpt_t_min   0.141
_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:
 N3(H3), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B), C7(H7A,H7B), C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C17(H17), C25(H25), C1(H1), C12(H12), C4(H4), C13(H13), C11(H11),
 C3(H3A), C14(H14), C2(H2A), C19(H19)
;
_shelx_res_checksum              19432
_olex2_submission_special_instructions 'No special instructions were received'