Assembling two Dy2 single-molecule magnets with different energy barriers via fine-tuning the geometries of DyIII sites
Li, Dawei; Ding, Man-Man; Ge, Yu; Tello Yepes, David Felipe; Sun, Mingyuan; Najib, Muhammad Saleem; Li, Yahong; Zhang, Yi-Quan; Yao, Jin-lei; New Journal of Chemistry 44 (2020) 20634–20642; doi:10.1039/D0NJ04009F

data_7060156
_publ_section_title
;
 Assembling two Dy2 single-molecule magnets with different energy barriers
 via fine-tuning the geometries of DyIII sites
;
_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20634
_journal_page_last               20642
_journal_paper_doi               10.1039/D0NJ04009F
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C37 H40 Cl2 Dy2 N5 O14, 2(C2 H6 O)'
_chemical_formula_sum            'C41 H52 Cl2 Dy2 N5 O16'
_chemical_formula_weight         1266.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-12 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1560(9)
_cell_length_b                   12.3704(5)
_cell_length_c                   16.9025(6)
_cell_measurement_reflns_used    9379
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.455
_cell_measurement_theta_min      2.410
_cell_volume                     4841.7(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0895
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16460
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         2.409
_exptl_absorpt_coefficient_mu    3.245
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1682 before and 0.0669 after correction. The Ratio of minimum to maximum transmission is 0.6828. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       block
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.223
_refine_ls_abs_structure_details
;
 Flack x determined using 3762 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10514
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0706P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1351
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_full    0.923
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                9234
_reflns_number_total             10514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04009f2.cif
_cod_data_source_block           t_CCDC1
_cod_database_code               7060156
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C31(H31A,H31B), C8(H8A,H8B), C24(H24A,H24B), C33(H33A,H33B),
 C36(H36A,H36B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C28(H28), C2(H2), C23(H23), C7(H7), C21(H21), C27(H27),
 C12(H12), C5(H5), C18(H18), C3(H3), C19(H19), C26(H26), C39(H39)
2.c Tetrahedral OH refined with riding coordinates:
 O16(H16)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C40(H40A,H40B,H40C), C37(H37A,H37B,H37C), C41(H41A,H41B,H41C)
2.e Idealised tetrahedral OH refined as rotating group:
 O15(H15)
;
_shelx_res_checksum              6988
_olex2_submission_special_instructions 'No special instructions were received'