Switching on single-molecule magnet properties of homoleptic sandwich tris(pyrazolyl)borate dysprosium(iii) cations via intermolecular dipolar coupling.
Alexandropoulos, Dimitris I.; Vignesh, Kuduva R.; Xie, Haomiao; Dunbar, Kim R.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10610–10618; doi:10.1039/c9dt00597h

data_7700048
_publ_section_title
;
 Switching on single-molecule magnet properties of homoleptic sandwich
 tris(pyrazolyl)borate dysprosium(iii) cations via intermolecular dipolar
 coupling.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10610
_journal_page_last               10618
_journal_paper_doi               10.1039/c9dt00597h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C30 H44 B2 Dy N12, C15 H22 B Cl3 Dy N6, C H2 Cl2'
_chemical_formula_sum            'C46 H68 B3 Cl5 Dy2 N18'
_chemical_formula_weight         1407.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc210f2l
_audit_creation_date             2018-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-05 deposited with the CCDC.    2019-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.5040(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2885(5)
_cell_length_b                   36.2677(19)
_cell_length_c                   16.0699(9)
_cell_measurement_reflns_used    9387
_cell_measurement_temperature    110
_cell_measurement_theta_max      25.722
_cell_measurement_theta_min      2.398
_cell_volume                     5990.6(5)
_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)'
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            195830
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.790
_diffrn_reflns_theta_max         25.790
_diffrn_reflns_theta_min         2.059
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.747
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0851 before and 0.0634 after correction. The Ratio of minimum to maximum transmission is 0.8509. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         11476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0244
_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/[\s^2^(Fo^2^)+(0.0093P)^2^+12.5212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0459
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10111
_reflns_number_total             11476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00597h2.cif
_cod_data_source_block           da1012_mecn_0m_a
_cod_depositor_comments
'Adding full bibliography for 7700048--7700050.cif.'
_cod_database_code               7700048
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.610
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3A)
2.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C18(H18), C23(H23), C28(H28), C33(H33), C38(H38),
 C43(H43)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              97394
_olex2_submission_special_instructions 'No special instructions were received'