Unusual undecanuclear heterobimetallic Zn4Ln7 (Ln = Gd, Dy) nano-sized clusters encapsulating two peroxide anions through spontaneous intake of dioxygen
Ke, Hongshan; Lu, Xiaohua; Wei, Wen; Wang, Wenyuan; Xie, Gang; Chen, Sanping; Dalton Trans.  (2017) –; doi:10.1039/C7DT01501A

data_7043316
_publ_section_title
;
 Unusual undecanuclear heterobimetallic Zn4Ln7 (Ln = Gd, Dy) nano-sized
 clusters encapsulating two peroxide anions through spontaneous intake of
 dioxygen
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01501A
_journal_year                    2017
_chemical_formula_moiety
'C112 H100 Cl4 Dy7 N8 O36 Zn4, Cl, 4(C2 H3 N)'
_chemical_formula_sum            'C120 H120 Cl5 Dy7 N12 O40 Zn4'
_chemical_formula_weight         3946.50
_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             2017-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-04-19 deposited with the CCDC.
2017-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                72.1550(10)
_cell_angle_beta                 75.1570(10)
_cell_angle_gamma                66.4450(10)
_cell_formula_units_Z            2
_cell_length_a                   16.2712(8)
_cell_length_b                   19.3688(9)
_cell_length_c                   27.8061(13)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    177(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.51
_cell_volume                     7556.2(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      177.15
_diffrn_measured_fraction_theta_full 0.989
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            38618
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.876
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.198
_exptl_absorpt_correction_T_max  0.511
_exptl_absorpt_correction_T_min  0.470
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       block
_exptl_crystal_F_000             3822
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.062
_refine_diff_density_min         -3.167
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1667
_refine_ls_number_reflns         26314
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0563
_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^)+(0.1043P)^2^+18.5935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19382
_reflns_number_total             26314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01501a2.cif
_cod_data_source_block           1_sq
_cod_database_code               7043316
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.519
_shelx_estimated_absorpt_t_min   0.420
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O28-H28E
 2 with sigma of 0.02
 H25A-H27A
 1.95 with sigma of 0.02
3.a Rotating group:
 O26(H26A,H26B), O27(H27A,H27B), O28(H28D,H28E), O25(H25A,H25B)
3.b Ternary CH refined with riding coordinates:
 O29(H29), O30(H30A), O35(H35A), O36(H36)
3.c Me refined with riding coordinates:
 C116(H11D,H11E,H11F)
3.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C24(H24), C25(H25), C26(H26),
  C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C38(H38), C39(H39),
 C40(H40), C44(H44), C45(H45), C46(H46), C47(H47), C49(H49), C52(H52), C53(H53),
  C54(H54), C58(H58), C59(H59), C60(H60), C61(H61), C63(H63), C66(H66),
 C67(H67), C68(H68), C72(H72), C73(H73), C74(H74), C75(H75), C77(H77), C80(H80),
  C81(H81), C82(H82), C86(H86), C87(H87), C88(H88), C89(H89), C91(H91),
 C94(H94), C95(H95), C96(H96), C100(H100), C101(H101), C102(H102), C103(H103),
 C105(H105), C108(H108), C109(H109), C110(H110)
3.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C42(H42A,H42B,H42C), C56(H56A,H56B,
 H56C), C70(H70A,H70B,H70C), C84(H84A,H84B,H84C), C98(H98A,H98B,H98C),
 C112(H11A,H11B,H11C), C120(H12A,H12B,H12C), C118(H11G,H11H,H11I), C114(H11J,
 H11K,H11L)
;
_shelx_res_checksum              2719
_shelx_fab_checksum              76634
_olex2_submission_special_instructions 'No special instructions were received'