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_7229678
_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         '2(C61 H54 Ho2 N6 O11), 2.5(C2 H3 N)'
_chemical_formula_sum            'C127 H115.5 Ho4 N14.5 O22'
_chemical_formula_weight         2856.55
_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                76.8060(10)
_cell_angle_beta                 72.9870(10)
_cell_angle_gamma                87.5900(10)
_cell_formula_units_Z            2
_cell_length_a                   16.0223(6)
_cell_length_b                   19.7955(7)
_cell_length_c                   20.3368(7)
_cell_measurement_reflns_used    9798
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.276
_cell_measurement_theta_min      3.067
_cell_volume                     6003.0(4)
_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 0.983
_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  0.0410
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            91179
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.347
_diffrn_reflns_theta_min         2.935
_exptl_absorpt_coefficient_mu    2.683
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0802 before and 0.0524 after correction.
The Ratio of minimum to maximum transmission is 0.7550.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       block
_exptl_crystal_F_000             2846
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.512
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1547
_refine_ls_number_reflns         29490
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+52.1315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20077
_reflns_number_total             29490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra11750g2.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C127 H115.50 Ho4 N14.50 O22'
_cod_database_code               7229678
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.705
_shelx_estimated_absorpt_t_min   0.454
_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
 O11-H11
 0.85 with sigma of 0.02
 O22-H22
 0.85 with sigma of 0.02
 N13-C124
 1.1 with sigma of 0.02
 C124-C123
 1.4 with sigma of 0.02
 N15-C128
 1 with sigma of 0.02
 C127-N15
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C124 \\sim C123 \\sim N13: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C127 \\sim C128 \\sim N15: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O12 \\sim C62: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O14) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C84)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C80) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C123) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N13) \\sim Ueq, Uanis(C124) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C127) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(N15) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C62) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: C128(0.5) C127(0.5) H12J(0.5) H12K(0.5) H12L(0.5) N15(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C89(H89), C17(H17), C10(H10), C71(H71), C28(H28), C59(H59), C15(H15),
 C88(H88), C76(H76), C112(H112), C16(H16), C50(H50), C33(H33), C72(H72),
 C111(H111), C11(H11A), C98(H98), C95(H95), C41(H41), C32(H32), C106(H106),
 C93(H93), C120(H120), C34(H34), C27(H27), C110(H110), C49(H49), C45(H45),
 C115(H115), C44(H44), C8(H8), C86(H86), C77(H77), C25(H25), C42(H42),
 C105(H105), C99(H99), C102(H102), C103(H103), C94(H94), C40(H40), C38(H38),
 C101(H101), C67(H67), C78(H78), C54(H54), C68(H68), C69(H69), C37(H37), C4(H4),
  C51(H51), C3(H3), C21(H21), C20(H20), C24(H24), C82(H82), C65(H65), C6(H6),
 C23(H23), C85(H85), C64(H64), C84(H84), C81(H81), C7(H7)
5.b Idealised Me refined as rotating group:
 C117(H11B,H11C,H11D), C56(H56A,H56B,H56C), C118(H11E,H11F,H11G), C96(H96A,
 H96B,H96C), C52(H52A,H52B,H52C), C122(H12A,H12B,H12C), C113(H11H,H11I,H11J),
 C57(H57A,H57B,H57C), C61(H61A,H61B,H61C), C18(H18A,H18B,H18C), C35(H35A,H35B,
 H35C), C62(H62A,H62B,H62C), C79(H79A,H79B,H79C), C1(H1A,H1B,H1C), C123(H12G,
 H12H,H12I), C125(H12D,H12E,H12F), C127(H12J,H12K,H12L)
;
_shelx_res_checksum              33081
_olex2_submission_special_instructions 'No special instructions were received'