A series of planar tetranuclear lanthanide complexes: axial ligand modulated magnetic dynamics in Dy4 species
Zhang, Ya-Xin; Li, Meng; Liu, Bi-Ying; Wu, Zhi-Lei; Wei, Hai-Ying; Wang, Wen-Min; RSC Advances 7 (2017) 55523–; doi:10.1039/C7RA11750G

data_7229679
_publ_section_title
;
 A series of planar tetranuclear lanthanide complexes: axial ligand
 modulated magnetic dynamics in Dy4 species
;
_journal_issue                   87
_journal_name_full               'RSC Advances'
_journal_page_first              55523
_journal_paper_doi               10.1039/C7RA11750G
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety
'C146 H156 Eu4 N12 O22, 2(C2 H3 N), 2(C2 H6 O)'
_chemical_formula_sum            'C154 H174 Eu4 N14 O24'
_chemical_formula_weight         3212.90
_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             2017-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-03 deposited with the CCDC.
2017-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                67.916(4)
_cell_angle_beta                 74.079(5)
_cell_angle_gamma                71.793(4)
_cell_formula_units_Z            1
_cell_length_a                   14.9764(8)
_cell_length_b                   16.0330(8)
_cell_length_c                   17.9785(10)
_cell_measurement_reflns_used    11075
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3739.1(4)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9407
              2theta: -15.0888
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9407
              2theta: -15.0888
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9407
              2theta: -15.0888
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.037788
_diffrn_orient_matrix_UB_12      0.023243
_diffrn_orient_matrix_UB_13      -0.055988
_diffrn_orient_matrix_UB_21      -0.022054
_diffrn_orient_matrix_UB_22      -0.062497
_diffrn_orient_matrix_UB_23      -0.020075
_diffrn_orient_matrix_UB_31      -0.047116
_diffrn_orient_matrix_UB_32      0.038702
_diffrn_orient_matrix_UB_33      -0.001865
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47942
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.567
_diffrn_reflns_theta_min         3.096
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1640
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.854
_refine_diff_density_min         -1.547
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         16871
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+6.0652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15235
_reflns_number_total             16871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra11750g2.cif
_cod_data_source_block           6
_cod_database_code               7229679
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.724
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H11 of O11, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H12A of O12
2. Restrained distances
 C63-C64 = C63-C65 = C63-C66 = C63-C64' = C63-C65' = C63-C66'
 1.54 with sigma of 0.01
 H77A-H66D
 2.2 with sigma of 0.02
 H77B-H66E
 2.2 with sigma of 0.02
 H77A-H66E
 2.2 with sigma of 0.02
3. Rigid bond restraints
 O9, C67
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O8, C58
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C64 \\sim C65 \\sim C66 \\sim C64' \\sim C65' \\sim C66': within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C76 \\sim C77: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C64')
\\sim Ueq, Uanis(C65') \\sim Ueq, Uanis(C66') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C76) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C64')=Sof(H64D)=Sof(H64E)=Sof(H64F)=Sof(C65')=Sof(H65D)=Sof(H65E)=
 Sof(H65F)=Sof(C66')=Sof(H66D)=Sof(H66E)=Sof(H66F)=1-FVAR(1)
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=
 Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 O11(H11)
6.b Secondary CH2 refined with riding coordinates:
 C76(H76A,H76B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C32(H32), C33(H33), C37(H37), C38(H38), C41(H41),
 C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C49(H49), C50(H50), C57(H57),
  C68(H68)
6.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C34(H34A,H34B,H34C), C51(H51A,H51B,H51C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C60(H60A,H60B,H60C), C61(H61A,
 H61B,H61C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C64'(H64D,H64E,H64F), C65'(H65D,H65E,H65F), C66'(H66D,
 H66E,H66F), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C),
 C75(H75A,H75B,H75C), C77(H77A,H77B,H77C)
6.e Idealised tetrahedral OH refined as rotating group:
 O12(H12A)
;
_shelx_res_checksum              24840
_olex2_submission_special_instructions 'No special instructions were received'