Hard versus soft: zero-field dinuclear Dy(iii) oxygen bridged SMM and theoretical predictions of the sulfur and selenium analogues.
Vignesh, Kuduva R.; Alexandropoulos, Dimitris I.; Dolinar, Brian S.; Dunbar, Kim R.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2872–2876; doi:10.1039/c9dt00324j

data_7048760
_publ_section_title
;
 Hard versus soft: zero-field dinuclear Dy(iii) oxygen bridged SMM and
 theoretical predictions of the sulfur and selenium analogues.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2872
_journal_page_last               2876
_journal_paper_doi               10.1039/c9dt00324j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'2(C23 H29 Gd N O7), 3(N O3), C6 H16 N, C2 H3 N'
_chemical_formula_sum            'C54 H77 Gd2 N7 O23'
_chemical_formula_weight         1506.72
_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   mixed
_audit_creation_date             2018-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-21 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.5460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.9973(9)
_cell_length_b                   12.6932(4)
_cell_length_c                   19.6403(6)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.44
_cell_measurement_theta_min      2.29
_cell_volume                     6212.7(3)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_diffrn_ambient_temperature      110.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            72413
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.455
_diffrn_reflns_theta_min         2.084
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.199
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1538 before and 0.0497 after correction. The Ratio of minimum to maximum transmission is 0.7737. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.017
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1204
_refine_ls_number_reflns         12791
_refine_ls_number_restraints     1244
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0182P)^2^+17.3633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10737
_reflns_number_total             12791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00324j2.cif
_cod_data_source_block           vig43_a
_cod_depositor_comments
'Adding full bibliography for 7048759--7048760.cif.'
_cod_database_code               7048760
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.473
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{O3A, O4}
3. Restrained distances
 O2-H2
 0.87 with sigma of 0.01
 O3-H3
 0.87 with sigma of 0.01
 O4-H4
 0.87 with sigma of 0.01
 O3A-H3AA
 0.87 with sigma of 0.005
 O1'-H1'
 0.87 with sigma of 0.01
 O3'-H3'
 0.87 with sigma of 0.01
 O4'-H4'
 0.87 with sigma of 0.01
 O2A-H2A
 0.87 with sigma of 0.01
 O1'A-H1'C
 0.87 with sigma of 0.01
 O4'A-H4'C
 0.87 with sigma of 0.01
 C4A-H2A
 1.928014 with sigma of 0.02
 Gd1-H2A
 2.950165 with sigma of 0.02
 C1'A-H1'C
 1.903229 with sigma of 0.02
 Gd1'-H1'C
 3.044958 with sigma of 0.02
 C8'A-H4'C
 1.914525 with sigma of 0.02
 Gd1'-H4'C
 2.721579 with sigma of 0.02
 N3-C24 \\sim N3-C24A \\sim N3-C26 \\sim N3-C26A \\sim N3-C28 \\sim N3-C28A
 with sigma of 0.02
 H4-O9 \\sim H3AA-O9
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim C1 \\sim C2 \\sim C3 \\sim C4
\\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim O1A \\sim O2A \\sim O3A \\sim O4A
\\sim O5A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A
\\sim C8A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
O3' \\sim O4' \\sim O5' \\sim C1' \\sim C2' \\sim C3' \\sim C4' \\sim C5' \\sim
C6' \\sim C7' \\sim C8' \\sim O1'A \\sim O2'A \\sim O3'A \\sim O4'A \\sim O5'A
\\sim C1'A \\sim C2'A \\sim C3'A \\sim C4'A \\sim C5'A \\sim C6'A \\sim C7'A
\\sim C8'A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C24A \\sim C25A
\\sim C26A \\sim C27A \\sim C28A \\sim C29A: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C9' \\sim C10' \\sim C11' \\sim C12' \\sim C13' \\sim C14' \\sim C9A \\sim C10A
\\sim C11A \\sim C12A \\sim C13A \\sim C14A: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C18' \\sim C19' \\sim C20' \\sim C21' \\sim C22' \\sim C23' \\sim C18A \\sim
C19A \\sim C20A \\sim C21A \\sim C22A \\sim C23A: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O4A) = Uanis(O1)
Uanis(O3A) = Uanis(O4)
5. Same fragment restrains
{O1A, O2A, O3A, O4A, O5A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A} sigma for
1-2: 0.04, 1-3: 0.08
{O1', O2', O3', O4', O5', C1', C2', C3', C4', C5', C6', C7', C8'} sigma for
1-2: 0.04, 1-3: 0.08
{O1'A, O2'A, O3'A, O4'A, O5'A, C1'A, C2'A, C3'A, C4'A, C5'A, C6'A, C7'A, C8'A}
sigma for 1-2: 0.04, 1-3: 0.08
as
{O1, O2, O3, O4, O5, C1, C2, C3, C4, C5, C6, C7, C8}
{C9A, C10A, C11A, C12A, C13A, C14A} sigma for 1-2: 0.02, 1-3: 0.04
{C18', C19', C20', C21', C22', C23'} sigma for 1-2: 0.02, 1-3: 0.04
{C18A, C19A, C20A, C21A, C22A, C23A} sigma for 1-2: 0.02, 1-3: 0.04
as
{C9', C10', C11', C12', C13', C14'}
{C24A, C25A, C26A, C27A, C28A, C29A} sigma for 1-2: 0.02, 1-3: 0.04
as
{C24, C25, C26, C27, C28, C29}
6. Others
 Sof(O1A)=Sof(H1AA)=Sof(O2A)=Sof(H2A)=Sof(O3A)=Sof(H3AA)=Sof(O4A)=Sof(O5A)=
 Sof(H5AA)=Sof(C1A)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(C3A)=Sof(H3AB)=Sof(H3AC)=
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=1-FVAR(1)
 Sof(O1)=Sof(O2)=Sof(H2)=Sof(O3)=Sof(H3)=Sof(O4)=Sof(H4)=Sof(O5)=Sof(H5)=
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=
 Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=FVAR(1)
 Sof(O1'A)=Sof(H1'C)=Sof(O2'A)=Sof(H2'A)=Sof(O3'A)=Sof(O4'A)=Sof(H4'C)=
 Sof(O5'A)=Sof(H5'C)=Sof(C1'A)=Sof(H1'D)=Sof(H1'E)=Sof(C2'A)=Sof(C3'A)=
 Sof(H3'C)=Sof(H3'D)=Sof(C4'A)=Sof(H4'D)=Sof(H4'E)=Sof(C5'A)=Sof(H5'D)=
 Sof(H5'E)=Sof(C6'A)=Sof(H6'C)=Sof(H6'D)=Sof(C7'A)=Sof(H7'C)=Sof(H7'D)=
 Sof(C8'A)=Sof(H8'C)=Sof(H8'D)=1-FVAR(2)
 Sof(O1')=Sof(H1')=Sof(O2')=Sof(O3')=Sof(H3')=Sof(O4')=Sof(H4')=Sof(O5')=
 Sof(H5')=Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(C2')=Sof(C3')=Sof(H3'A)=Sof(H3'B)=
 Sof(C4')=Sof(H4'A)=Sof(H4'B)=Sof(C5')=Sof(H5'A)=Sof(H5'B)=Sof(C6')=Sof(H6'A)=
 Sof(H6'B)=Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(C8')=Sof(H8'A)=Sof(H8'B)=FVAR(2)
 Sof(H3BE)=Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C25A)=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=1-FVAR(3)
 Sof(H3AD)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(3)
 Sof(C18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=1-FVAR(4)
 Sof(C18')=Sof(C19')=Sof(H19')=Sof(C20')=Sof(H20')=Sof(C21')=Sof(H21')=
 Sof(C22')=Sof(H22')=Sof(C23')=Sof(H23')=FVAR(4)
 Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=
 Sof(C13A)=Sof(H13A)=Sof(C14A)=1-FVAR(5)
 Sof(C9')=Sof(H9')=Sof(C10')=Sof(H10')=Sof(C11')=Sof(H11')=Sof(C12')=Sof(H12')=
 Sof(C13')=Sof(H13')=Sof(C14')=FVAR(5)
7.a Ternary CH refined with riding coordinates:
 N3(H3AD), N3(H3BE)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C1A(H1AB,H1AC), C3A(H3AB,H3AC), C4A(H4AA,H4AB), C5A(H5AB,H5AC),
 C6A(H6AA,H6AB), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C1'(H1'A,H1'B), C3'(H3'A,H3'B),
  C4'(H4'A,H4'B), C5'(H5'A,H5'B), C6'(H6'A,H6'B), C7'(H7'A,H7'B), C8'(H8'A,
 H8'B), C1'A(H1'D,H1'E), C3'A(H3'C,H3'D), C4'A(H4'D,H4'E), C5'A(H5'D,H5'E),
 C6'A(H6'C,H6'D), C7'A(H7'C,H7'D), C8'A(H8'C,H8'D), C24(H24A,H24B), C26(H26A,
 H26B), C28(H28A,H28B), C24A(H24C,H24D), C26A(H26C,H26D), C28A(H28C,H28D)
7.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23), C16'(H16'), C9'(H9'), C10'(H10'), C11'(H11'),
 C12'(H12'), C13'(H13'), C19'(H19'), C20'(H20'), C21'(H21'), C22'(H22'),
 C23'(H23'), C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A),
 C19A(H19A), C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A)
7.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C25A(H25D,H25E,
 H25F), C27A(H27D,H27E,H27F), C29A(H29D,H29E,H29F), C31(H31A,H31B,H31C)
7.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O1A(H1AA), O5A(H5AA), O5'(H5'), O2'A(H2'A), O5'A(H5'C)
;
_shelx_res_checksum              75735
_olex2_submission_special_instructions 'No special instructions were received'