Effect of coordination anion substitutions on relaxation dynamics of defect dicubane Zn<sub>2</sub>Dy<sub>2</sub> tetranuclear clusters.
Ke, Hongshan; Wei, Wen; Yang, Yongsheng; Zhang, Jun; Zhang, Yi-Quan; Xie, Gang; Chen, Sanping; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7844–7852; doi:10.1039/c9dt01074b

data_7701578
_publ_section_title
;
 Effect of coordination anion substitutions on relaxation dynamics of
 defect dicubane Zn<sub>2</sub>Dy<sub>2</sub> tetranuclear clusters.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7844
_journal_page_last               7852
_journal_paper_doi               10.1039/c9dt01074b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C80 H94 Dy2 N4 O18 Zn2, 4(C3 H6 O)'
_chemical_formula_sum            'C92 H118 Dy2 N4 O22 Zn2'
_chemical_formula_weight         2087.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-23
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.04.18 svn.r3594 for OlexSys, GUI svn.r5739)
;
_audit_update_record
;
2019-04-23 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                70.194(4)
_cell_angle_beta                 70.908(4)
_cell_angle_gamma                62.195(4)
_cell_formula_units_Z            1
_cell_length_a                   12.903(3)
_cell_length_b                   13.716(3)
_cell_length_c                   15.560(3)
_cell_measurement_reflns_used    2672
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.03
_cell_measurement_theta_min      2.53
_cell_volume                     2244.0(8)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'SAINT v7.34A (Bruker, 200?)'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.1512
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14174
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.146
_diffrn_reflns_theta_min         1.421
_exptl_absorpt_coefficient_mu    2.248
_exptl_absorpt_correction_T_max  0.6879
_exptl_absorpt_correction_T_min  0.6552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       block
_exptl_crystal_F_000             1066
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.497
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         8843
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0503P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5850
_reflns_number_total             8843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01074b2.cif
_cod_data_source_block           2
_cod_database_code               7701578
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.688
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O10-C44 = O10A-C44A
 1.2 with sigma of 0.01
 C45A-C44A = C46A-C44A = C46-C44 = C45-C44
 1.5 with sigma of 0.01
 O10A_$1-O7
 2.91 with sigma of 0.001
 C39-H9A
 1.882913 with sigma of 0.02
 Zn1-H9A
 2.695258 with sigma of 0.02
 O10-C45 \\sim O10-C46 \\sim O10A-C45A \\sim O10A-C46A
 with sigma of 0.02
3. Restrained planarity
 O10A, C44A, C45A, C46A
 with sigma of 0.1
 O10, C44, C45, C46
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C44) = Uanis(C44A)
Uanis(C45) = Uanis(C45A)
Uanis(C46) = Uanis(C46A)
Uanis(O10A) = Uanis(O10)
5. Rigid body (RIGU) restrains
 O10A, C44A, C45A, C46A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O10, C44, C45, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Others
 Sof(O10A)=Sof(C44A)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C46A)=
 Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(1)
 Sof(O10)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46)=Sof(H46A)=Sof(H46B)=
 Sof(H46C)=Sof(C44)=FVAR(1)
7.a Riding coordinates:
 O9(H9A), C46A(H46D,H46E,H46F)
7.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B)
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), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C45A(H45D,H45E,
 H45F)
;
_shelx_res_checksum              405
_olex2_submission_special_instructions 'No special instructions were received'