Two {ZnII2DyIII} complexes supported by monophenoxido/dicarboxylates bridges with multiple relaxation processes: carboxylato ancillary ligands controlled magnetic anisotropy in square antiprismatic DyIII species
Li, Min; Wu, Haipeng; Wei, Qing; Ke, Hongshan; Yin, Bing; Zhang, Sheng; Lv, Xingqiang; Xie, Gang; Chen, Sanping; Dalton Transactions  (2018) –; doi:10.1039/C8DT01842A

data_7046712
_publ_section_title
;
 Two {ZnII2DyIII} complexes supported by monophenoxido/dicarboxylates
 bridges with multiple relaxation processes: carboxylato ancillary ligands
 controlled magnetic anisotropy in square antiprismatic DyIII species
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT01842A
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C46 H40 Dy N6 O14 Zn2), 2(C7 H5 O2)'
_chemical_formula_sum            'C106 H90 Dy2 N12 O32 Zn4'
_chemical_formula_weight         2630.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-15 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.737(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.333(5)
_cell_length_b                   10.771(2)
_cell_length_c                   27.313(6)
_cell_measurement_reflns_used    4041
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.781
_cell_measurement_theta_min      2.372
_cell_volume                     6010(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30261
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.557
_exptl_absorpt_coefficient_mu    2.090
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0858 before and 0.0603 after correction. The Ratio of minimum to maximum transmission is 0.7840. The \l/2 correction factor is 0.0015.'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             2636
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.025(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1374
_refine_ls_number_reflns         20328
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                13033
_reflns_number_total             20328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01842a2.cif
_cod_data_source_block           DZ_1
_cod_database_code               7046712
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.759
_shelx_estimated_absorpt_t_min   0.705
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.975(18)
 0.025(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C104-C105
 1.4 with sigma of 0.02
 C70-C75
 1.45 with sigma of 0.01
 C77-C82
 1.49 with sigma of 0.02
 C98-C111
 1.45 with sigma of 0.01
 C36-C41
 1.4 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C36, C41, C37, C40, C38, C39, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C108, O32, C104, O31, C105, C107, C110, C106, C109
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C23, C22, C27, C26, C25, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O29, O30, C103, C98, C111, C101, C100, C99, C102, O31, C104, O32, C110, C109,
 C108, C106, C107, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C73, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C93, C94
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C44, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 N8(H8A), C18(H18), N2(H2), N5(H5), C72(H72), N11(H11), C71(H71), C31(H31),
 C3(H3), C56(H56), C8(H8), C78(H78), C4(H4), C51(H51), C73(H73), C32(H32),
 C82(H82), C5(H5A), C85(H85), C96(H96), C80(H80), C33(H33), C79(H79), C30(H30),
 C41(H41), C95(H95), C74(H74), C66(H66), C89(H89), C37(H37), C34(H34), C53(H53),
  C81(H81), C92(H92), C86(H86), C61(H61), C75(H75), C88(H88), C52(H52),
 C94(H94), C93(H93), C40(H40), C13(H13), C38(H38), C87(H87), C14(H14), C15(H15),
  C39(H39), C63(H63), C62(H62), C26(H26), C25(H25), C24(H24), C23(H23),
 C27(H27), C45(H45), C46(H46), C48(H48), C44(H44), C47(H47), C111(H111),
 C101(H101), C100(H100), C99(H99), C102(H102), C107(H107), C106(H106),
 C108(H108), C109(H109), C110(H110)
6.b Fitted hexagon refined as free rotating group:
 C26(C25,C24,C23,C22,C27), C45(C46,C48,C43,C44,C47), C105(C107,C106,C108,C109,
 C110)
6.c X=CH2 refined with riding coordinates:
 N6(H6A,H6B), N3(H3A,H3B), N12(H12A,H12B), N9(H9A,H9B)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C59(H59A,H59B,H59C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              1328
_shelx_fab_checksum              51842
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'