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_7229676
_publ_section_title
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 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         'C142 H116 Dy4 N12 O22, 4(C2 H3 N)'
_chemical_formula_sum            'C150 H128 Dy4 N16 O22'
_chemical_formula_weight         3156.68
_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
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 103.736(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.423(3)
_cell_length_b                   13.940(2)
_cell_length_c                   30.573(6)
_cell_measurement_reflns_used    6953
_cell_measurement_temperature    386(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      3.0
_cell_volume                     7213(2)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      386.3
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            60491
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.002
_exptl_absorpt_coefficient_mu    2.119
_exptl_absorpt_correction_T_max  0.8525
_exptl_absorpt_correction_T_min  0.5647
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         2.552
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         12620
_refine_ls_number_restraints     296
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0885
_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^)+(0.1158P)^2^+39.6652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7998
_reflns_number_total             12620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra11750g2.cif
_cod_data_source_block           10
_cod_database_code               7229676
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.524
_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
 C25-C22
 1.45 with sigma of 0.02
 C74-C75
 1.57 with sigma of 0.02
 H18A-H24
 2.2 with sigma of 0.02
 H34_$1-H74C_$2
 2.2 with sigma of 0.02
 H72B-H74A
 2.2 with sigma of 0.02
 H74B-H72B
 2.2 with sigma of 0.02
3. Rigid bond restraints
 Dy2, O11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O3, C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C58, C59, C55
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C58 \\sim C55 \\sim C59 \\sim C57 \\sim C56 \\sim C54 \\sim C53 \\sim C52:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
O3 \\sim C19 \\sim C18 \\sim C20: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O6) \\sim
Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C59) \\sim Ueq,
Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N7) \\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(C74) \\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C58) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C75) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C64(H64), C67(H67), C17(H17), C68(H68), C8(H8), C69(H69), C51(H51), C42(H42),
 C11(H11A), C71(H71), C10(H10), C49(H49), C70(H70), C4(H4), C3(H3), C7(H7),
 C6(H6), C28(H28), C50(H50), C44(H44), C38(H38), C45(H45), C41(H41), C27(H27),
 C15(H15), C40(H40), C37(H37), C25(H25), C59(H59), C16(H16), C21(H21), C23(H23),
  C24(H24), C20(H20), C53(H53), C52(H52), C57(H57), C56(H56), C54(H54),
 C32(H32), C33(H33), C34(H34)
5.b Fitted hexagon refined as free rotating group:
 C5(C4,C3,C2,C7,C6), C21(C22,C23,C24,C19,C20), C53(C52,C57,C56,C55,C54)
5.c Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C35(H35A,H35B,H35C), C1(H1A,H1B,H1C), C18(H18A,H18B,
 H18C), C62(H62A,H62B,H62C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              22691
_olex2_submission_special_instructions 'No special instructions were received'