Transitions of two magnetic interaction states in dinuclear Dy(iii) complexes via subtle structural variations.
Zhang, Kun; Liu, Dan; Vieru, Veacheslav; Hou, Lei; Cui, Bin; Guo, Fu-Sheng; Chibotaru, Liviu F.; Wang, Yao-Yu; Dalton transactions (Cambridge, England : 2003) 46 (2017) 638–642; doi:10.1039/c6dt04490e

data_7041323
_publ_section_title
;
 Transitions of two magnetic interaction states in dinuclear Dy(iii)
 complexes via subtle structural variations.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              638
_journal_page_last               642
_journal_paper_doi               10.1039/c6dt04490e
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
'C66 H62 Dy2 N4 O12, 2(C4 H9 N O), 2(C2 H3 N)'
_chemical_formula_sum            'C78 H86 Dy2 N8 O14'
_chemical_formula_weight         1684.54
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-14 deposited with the CCDC.
2016-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.805(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.2155(6)
_cell_length_b                   12.4815(4)
_cell_length_c                   17.6745(6)
_cell_measurement_reflns_used    6159
_cell_measurement_temperature    100.06(13)
_cell_measurement_theta_max      28.7240
_cell_measurement_theta_min      3.8300
_cell_volume                     3635.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.06(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_details
;
  1 omega  -21.00   78.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   19.0000  -30.0000 99

  2 omega   14.00   81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   19.0000   60.0000 67

  3 omega   66.00   92.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  178.0000   90.0000 26

  4 omega  -88.00  -49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663 -178.0000  -30.0000 39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0232515000
_diffrn_orient_matrix_UB_12      0.0451244000
_diffrn_orient_matrix_UB_13      -0.0176408000
_diffrn_orient_matrix_UB_21      0.0317352000
_diffrn_orient_matrix_UB_22      0.0164120000
_diffrn_orient_matrix_UB_23      -0.0156010000
_diffrn_orient_matrix_UB_31      -0.0175159000
_diffrn_orient_matrix_UB_32      -0.0303355000
_diffrn_orient_matrix_UB_33      -0.0346861000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16724
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.342
_diffrn_reflns_theta_min         3.457
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.754
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         8225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0350P)^2^+3.9607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6341
_reflns_number_total             8225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04490e2.cif
_cod_data_source_block           dy
_cod_depositor_comments
'Adding full bibliography for 7041323--7041324.cif.'
_cod_database_code               7041323
_chemical_oxdiff_formula         'C78 H86 Dy2 N8 O14'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C)
;
_shelx_res_checksum              75802
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'