Influence of alcoholic solvent and acetate anion coordination mode variations on structures and magnetic properties of heterometallic Zn<sub>2</sub>Dy<sub>2</sub> tetranuclear clusters.
Ke, Hongshan; Wei, Wen; Zhang, Yi-Quan; Zhang, Jun; Xie, Gang; Chen, Sanping; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16616–16626; doi:10.1039/c8dt03983f

data_7048029
_publ_section_title
;
 Influence of alcoholic solvent and acetate anion coordination mode
 variations on structures and magnetic properties of heterometallic
 Zn<sub>2</sub>Dy<sub>2</sub> tetranuclear clusters.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16616
_journal_page_last               16626
_journal_paper_doi               10.1039/c8dt03983f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C80 H94 Dy2 N4 O18 Zn2, 2(C H2 Cl2), 0.5(H2 O)'
_chemical_formula_sum            'C82 H99 Cl4 Dy2 N4 O18.5 Zn2'
_chemical_formula_weight         2034.19
_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
_audit_creation_date             2018-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-26 deposited with the CCDC.
2018-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                103.901(3)
_cell_angle_beta                 101.012(3)
_cell_angle_gamma                117.443(3)
_cell_formula_units_Z            1
_cell_length_a                   13.1780(15)
_cell_length_b                   13.6064(15)
_cell_length_c                   15.8544(17)
_cell_measurement_reflns_used    3123
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.59
_cell_measurement_theta_min      2.29
_cell_volume                     2293.9(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.973
_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  0.0600
_diffrn_reflns_av_unetI/netI     0.0964
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22939
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.522
_diffrn_reflns_theta_min         1.413
_exptl_absorpt_coefficient_mu    2.307
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0940 before and 0.0564 after correction. The Ratio of minimum to maximum transmission is 0.7599. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       plate
_exptl_crystal_F_000             1027
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;

;
_refine_diff_density_max         0.788
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         10283
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7606
_reflns_number_total             10283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03983f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7048029--7048030.cif.'
_cod_original_cell_volume        2293.9(4)
_cod_original_formula_sum        'C82 H99 Cl4 Dy2 N4 O18.50 Zn2'
_cod_database_code               7048029
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.596
_shelx_estimated_absorpt_t_min   0.544
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O9-H9A
 0.85 with sigma of 0.02
 C35A-C33 = C35-C33 = C34A-C33 = C34-C33 = C36A-C33 = C36-C33
 1.5 with sigma of 0.01
 C40-C39 = C40A-C39
 1.5 with sigma of 0.01
3. Rigid bond restraints
 C33, C35
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C33 \\sim C34 \\sim C35 \\sim C36 \\sim C35A \\sim C34A \\sim C36A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C39 \\sim C40 \\sim C40A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C36A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C40A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C33, C34, C35, C36, C35A, C34A, C36A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C39, C40, C40A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=
 Sof(H34F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
 Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(2)
 Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(2)
 Fixed Sof: O16(0.25) H16D(0.25) H16E(0.25)
 Fixed U11: O16(0.068305)
 Fixed U12: O16(0.028753)
 Fixed U13: O16(0.071036)
 Fixed U22: O16(0.099804)
 Fixed U23: O16(0.081991)
 Fixed U33: O16(0.13224)
 Fixed X: O16(0.1444)
 Fixed Y: O16(0.54876)
 Fixed Z: O16(0.663351)
7.a Riding coordinates:
 O16(H16D,H16E)
7.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C39(H39C,H39D), C41(H41A,H41B)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13), C22(H22),
 C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C31(H31)
7.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C35A(H35D,H35E,H35F),
 C34A(H34D,H34E,H34F), C36A(H36D,H36E,H36F), C40A(H40D,H40E,H40F)
;
_shelx_res_checksum              85227
_olex2_submission_special_instructions 'No special instructions were received'