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_7229674
_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 N12 O22 Tb4, 2(C2 H3 N), 2(C2 H6 O)'
_chemical_formula_sum            'C154 H174 N14 O24 Tb4'
_chemical_formula_weight         3240.74
_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             2017-08-19
_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                67.936(4)
_cell_angle_beta                 74.001(6)
_cell_angle_gamma                71.656(5)
_cell_formula_units_Z            1
_cell_length_a                   14.9673(6)
_cell_length_b                   15.9870(6)
_cell_length_c                   17.9639(8)
_cell_measurement_reflns_used    11445
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3720.2(3)
_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 0.991
_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: 44.9753
              2theta: -15.0921
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: 44.9753
              2theta: -15.0921
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: 44.9753
              2theta: -15.0921
;
_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      -0.053791
_diffrn_orient_matrix_UB_12      0.013846
_diffrn_orient_matrix_UB_13      -0.045092
_diffrn_orient_matrix_UB_21      -0.031368
_diffrn_orient_matrix_UB_22      -0.006038
_diffrn_orient_matrix_UB_23      0.061695
_diffrn_orient_matrix_UB_31      0.029548
_diffrn_orient_matrix_UB_32      0.053403
_diffrn_orient_matrix_UB_33      -0.001518
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41002
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.100
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.950
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1648
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.372
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         12988
_refine_ls_number_restraints     641
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0414P)^2^+6.1076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11703
_reflns_number_total             12988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra11750g2.cif
_cod_data_source_block           8
_cod_database_code               7229674
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.696
_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
 H11-O11
 0.85 with sigma of 0.02
 H66D-H75C
 2.2 with sigma of 0.02
 H75B-H66F
 2.2 with sigma of 0.02
 C74-O12
 1 with sigma of 0.02
 H66D-H75B
 2.2 with sigma of 0.02
3. 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
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. 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)
5.a Ternary CH refined with riding coordinates:
 O11(H11)
5.b Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B)
5.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)
5.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),
 C77(H77A,H77B,H77C), C75(H75A,H75B,H75C)
5.e Idealised tetrahedral OH refined as rotating group:
 O12(H12A)
;
_shelx_res_checksum              92417
_olex2_submission_special_instructions 'No special instructions were received'