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_7229677
_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 Dy4 N12 O22, 4(C2 H3 N)'
_chemical_formula_sum            'C154 H168 Dy4 N16 O22'
_chemical_formula_weight         3245.03
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-08-25
_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                68.0810(10)
_cell_angle_beta                 73.9990(10)
_cell_angle_gamma                71.2970(10)
_cell_formula_units_Z            1
_cell_length_a                   15.0463(5)
_cell_length_b                   15.9891(6)
_cell_length_c                   17.9493(6)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.312
_cell_measurement_theta_min      3.094
_cell_volume                     3734.3(2)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45210
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.006
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_min         2.935
_exptl_absorpt_coefficient_mu    2.049
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0733 before and 0.0433 after correction.
The Ratio of minimum to maximum transmission is 0.7554.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.412
_refine_diff_density_min         -1.511
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         13083
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0510P)^2^+17.1520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11031
_reflns_number_total             13083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra11750g2.cif
_cod_data_source_block           9
_cod_database_code               7229677
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.534
_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. Restrained distances
 C71B-C72B
 2.5 with sigma of 0.02
 C72A-C73A
 2.2 with sigma of 0.02
 H11-O11
 0.85 with sigma of 0.02
 C71B-C70 \\sim C70-C71A
 with sigma of 0.02
 C72A-C70 \\sim C70-C72B
 with sigma of 0.02
 C73B-C70 \\sim C70-C73A
 with sigma of 0.02
3. Rigid bond restraints
 C17, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C75) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C72A) \\sim Ueq, Uanis(C72B) \\sim Ueq, Uanis(C73B) \\sim Ueq,
Uanis(C71B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C71B) = Uanis(C71A)
Uanis(C73B) = Uanis(C73A)
Uanis(C72B) = Uanis(C72A)
5. Others
 Sof(C71B)=Sof(H71A)=Sof(H71B)=Sof(H71C)=1-FVAR(1)
 Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=FVAR(1)
 Sof(C72B)=Sof(H72A)=Sof(H72B)=Sof(H72C)=1-FVAR(2)
 Sof(C72A)=Sof(H72D)=Sof(H72E)=Sof(H72F)=FVAR(2)
 Sof(C73B)=Sof(H73A)=Sof(H73B)=Sof(H73C)=1-FVAR(3)
 Sof(C73A)=Sof(H73D)=Sof(H73E)=Sof(H73F)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C51(H51), C44(H44), C24(H24), C27(H27), C57(H57), C45(H45), C41(H41),
 C28(H28), C49(H49), C68(H68), C15(H15), C11(H11A), C16(H16), C10(H10),
 C33(H33), C42(H42), C37(H37), C4(H4), C23(H23), C25(H25), C32(H32), C34(H34),
 C6(H6), C3(H3), C8(H8), C38(H38), C40(H40), C17(H17), C21(H21), C50(H50),
 C20(H20), C1A(H1AA)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C54(H54A,H54B,H54C), C53(H53A,H53B,H53C), C52(H52A,H52B,
 H52C), C64(H64A,H64B,H64C), C1(H1A,H1B,H1C), C65(H65A,H65B,H65C), C35(H35A,
 H35B,H35C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C62(H62A,H62B,H62C),
 C60(H60A,H60B,H60C), C72B(H72A,H72B,H72C), C73B(H73A,H73B,H73C), C71B(H71A,
 H71B,H71C), C76(H76A,H76B,H76C), C74(H74A,H74B,H74C), C73A(H73D,H73E,H73F),
 C72A(H72D,H72E,H72F), C71A(H71D,H71E,H71F)
;
_shelx_res_checksum              39067
_olex2_submission_special_instructions 'No special instructions were received'