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_7043317
_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 Gd7 N8 O36 Zn4, 4(C2 H3 N), Cl'
_chemical_formula_sum            'C120 H120 Cl5 Gd7 N12 O40 Zn4'
_chemical_formula_weight         3909.75
_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                71.9570(10)
_cell_angle_beta                 75.9180(10)
_cell_angle_gamma                66.9010(10)
_cell_formula_units_Z            2
_cell_length_a                   16.0223(13)
_cell_length_b                   19.4348(14)
_cell_length_c                   27.978(2)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    177(2)
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      2.33
_cell_volume                     7545.3(10)
_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)'
_diffrn_ambient_temperature      177.15
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.977
_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  0.0436
_diffrn_reflns_av_unetI/netI     0.1064
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            41093
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.978
_diffrn_reflns_theta_min         1.552
_exptl_absorpt_coefficient_mu    3.815
_exptl_absorpt_correction_T_max  0.57
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       block
_exptl_crystal_F_000             3794
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.535
_refine_diff_density_min         -3.761
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1705
_refine_ls_number_reflns         28920
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0635P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17615
_reflns_number_total             28920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01501a2.cif
_cod_data_source_block           1_sq
_cod_original_cell_volume        7545.4(10)
_cod_database_code               7043317
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.547
_shelx_estimated_absorpt_t_min   0.474
_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
 H36-O36
 0.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N10) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Rotating group:
 O25(H25A,H25B), O26(H26A,H26B), O27(H27A,H27B), O28(H28D,H28E)
4.b Ternary CH refined with riding coordinates:
 O29(H29), O35(H35A)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C11(H11), C12(H12), C13(H13),
 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), C45(H45), C46(H46), C47(H47), C49(H49), C52(H52), C53(H53), C54(H54),
  C59(H59), C60(H60), C61(H61), C63(H63), C66(H66), C67(H67), C68(H68),
 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)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C42(H42A,H42B,H42C), C56(H56A,H56B,H56C), C70(H70A,H70B,
 H70C), C84(H84A,H84B,H84C), C98(H98A,H98B,H98C), C112(H11A,H11B,H11C),
 C114(H11D,H11E,H11F), C118(H11G,H11H,H11I), C116(H11J,H11K,H11L)
;
_shelx_res_checksum              70236
_shelx_fab_checksum              50848
_olex2_submission_special_instructions 'No special instructions were received'