Self-assembly of a unique 3d/4f heterometallic square prismatic box-like coordination cage.
Li, Li; Zhang, Yingjie; Avdeev, Maxim; Lindoy, Leonard F.; Harman, David G.; Zheng, Rongkun; Cheng, Zhenxiang; Aldrich-Wright, Janice R; Li, Feng; Dalton transactions (Cambridge, England : 2003) 45 (2016) 9407–9411; doi:10.1039/c6dt01651k

data_7040226
_publ_section_title
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 Self-assembly of a unique 3d/4f heterometallic square prismatic box-like
 coordination cage.
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_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9407
_journal_page_last               9411
_journal_paper_doi               10.1039/c6dt01651k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C152 H200 Cu6 Dy8 N80 O12, 6(O), 9(C H4 O)'
_chemical_formula_sum            'C161 H236 Cu6 Dy8 N80 O27'
_chemical_formula_weight         5405.52
_chemical_name_systematic
;
 ?
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_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-05-17 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90.01(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.673(12)
_cell_length_b                   42.718(9)
_cell_length_c                   24.298(5)
_cell_measurement_reflns_used    18000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.754
_cell_measurement_theta_min      0.953
_cell_volume                     25610(15)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       '\p  scans'
_diffrn_radiation_type
'silicon double crystal monochromated synchrotron'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            155733
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.754
_diffrn_reflns_theta_min         0.953
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    2.854
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       prism
_exptl_crystal_F_000             10720
_exptl_crystal_size_max          0.1010
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.514
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.000273(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1286
_refine_ls_number_reflns         21649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0945P)^2^+322.3011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16971
_reflns_number_total             21649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01651k2.cif
_cod_data_source_block           c2byc
_cod_database_code               7040226
_shelxl_version_number           2014-3
_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, All O(H,H) groups
2. Others
 Fixed Sof: O14(0.5) O18(0.5) O15(0.5) O19(0.5) O13(0.5) H13(0.5) C81(0.5)
 H81A(0.5) H81B(0.5) H81C(0.5)
3.a Rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C7(H7A,H7B), C8(H8A,H8B), C13(H13A,H13B), C14(H14A,
 H14B), C20(H20A,H20B), C21(H21A,H21B), C26(H26A,H26B), C27(H27A,H27B),
 C32(H32A,H32B), C33(H33A,H33B), C39(H39A,H39B), C40(H40A,H40B), C45(H45A,H45B),
  C46(H46A,H46B), C51(H51A,H51B), C52(H52A,H52B), C58(H58A,H58B), C59(H59A,
 H59B), C64(H64A,H64B), C65(H65A,H65B), C70(H70A,H70B), C71(H71A,H71B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C9(H9), C11(H11), C12(H12), C15(H15), C17(H17),
 C18(H18), C22(H22), C24(H24), C25(H25), C28(H28), C30(H30), C31(H31), C34(H34),
  C36(H36), C37(H37), C41(H41), C43(H43), C44(H44), C47(H47), C49(H49),
 C50(H50), C53(H53), C55(H55), C56(H56), C60(H60), C62(H62), C63(H63), C66(H66),
  C68(H68), C69(H69), C72(H72), C74(H74), C75(H75)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C38(H38A,H38B,H38C), C57(H57A,H57B,H57C), C76(H76A,H76B,
 H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,
 H80B,H80C), C81(H81A,H81B,H81C)
3.e Idealised tetrahedral OH refined as rotating group:
 O9(H9A), O10(H10), O11(H11A), O12(H12A), O13(H13)
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_shelx_res_checksum              24382
_olex2_submission_special_instructions 'No special instructions were received'