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_7046713
_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_formula_moiety         'C26 H32 Dy N6 O14 Zn2, 2(C2 H3 O2)'
_chemical_formula_sum            'C32 H38 Dy N4 O18 Zn2'
_chemical_formula_weight         1059.90
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n'
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-15
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2398(17)
_cell_length_b                   14.2398(17)
_cell_length_c                   18.844(2)
_cell_measurement_reflns_used    3264
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.69
_cell_measurement_theta_min      2.29
_cell_volume                     3821.0(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22174
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.640
_diffrn_reflns_theta_min         2.023
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.264
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0867 before and 0.0507 after correction. The Ratio of minimum to maximum transmission is 0.8808. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.650
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4412
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0552
_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^)+(0.1170P)^2^+4.5071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2831
_reflns_number_total             4412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01842a2.cif
_cod_data_source_block           DZ_2
_cod_original_cell_volume        3820.9(10)
_cod_database_code               7046713
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.695
_shelx_estimated_absorpt_t_min   0.591
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C17-C18
 1.502 with sigma of 0.02
 C17-O10
 1.258 with sigma of 0.02
 C17-O11
 1.261 with sigma of 0.02
 H8-H18C
 2.2 with sigma of 0.02
 O10_$1-O10
 3.5 with sigma of 0.02
 O10-O11
 2.193 with sigma of 0.04
 O10-C18
 2.381 with sigma of 0.04
 C18-O11
 2.394 with sigma of 0.04
 Dy1-O5 \\sim Dy1-O5A
 with sigma of 0.02
 Zn1-O4 \\sim Zn1-O4A
 with sigma of 0.02
 O4-C11 \\sim O4A-C11A
 with sigma of 0.02
 O5-C11 \\sim O5A-C11A
 with sigma of 0.02
 C11-C12 \\sim C11A-C12A
 with sigma of 0.02
 Dy1-C11 \\sim Dy1-C11A
 with sigma of 0.04
 Zn1-C11 \\sim Zn1-C11A
 with sigma of 0.04
 O4-O5 \\sim O4A-O5A
 with sigma of 0.04
 O4-C12 \\sim O4A-C12A
 with sigma of 0.04
 O5-C12 \\sim O5A-C12A
 with sigma of 0.04
3. Restrained planarity
 O10, O11, C17, C18
 with sigma of 0.1
4. Rigid bond restraints
 C10, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O10 \\sim O11 \\sim C17 \\sim C18: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C12A) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O5A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.005
Uanis(O10) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(O11)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 O10, O11, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5A, O4A, C11A, C12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, O5, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O4A)=Sof(O5A)=Sof(C11A)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(O4)=Sof(O5)=Sof(C11)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
8.a Rotating group:
 N3(H3A,H3B)
8.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C8(H8), C5(H5), C3(H3), C4(H4)
8.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C12(H12A,H12B,
 H12C), C12A(H12D,H12E,H12F)
;
_shelx_res_checksum              1100
_olex2_submission_special_instructions 'No special instructions were received'