Bottom-Up Construction of POM-Based Macrostructures: Coordination Assembled Paddle-Wheel Macroclusters and Their Vesicle-like Supramolecular Aggregation in Solution
Yi Zhu; Panchao Yin; Fengping Xiao; Dong Li; Emily Bitterlich; Zicheng Xiao; Jin Zhang; Jian Hao; Tianbo Liu; Yuan Wang; Yongge Wei; Journal of the American Chemical Society 135 (2013) 17155–17160; doi:10.1021/ja408228b

data_4121124
_publ_section_title
;
 Bottom-Up Construction of POM-Based Macrostructures: Coordination
 Assembled Paddle-Wheel Macroclusters and Their Vesicle-like
 Supramolecular Aggregation in Solution
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17155
_journal_page_last               17160
_journal_paper_doi               10.1021/ja408228b
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C337 H655.5 Cu4 Mo48 N34.5 O164'
_chemical_formula_weight         12674.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.4350(10)
_cell_angle_beta                 91.753(2)
_cell_angle_gamma                102.066(2)
_cell_formula_units_Z            2
_cell_length_a                   27.362(3)
_cell_length_b                   29.399(4)
_cell_length_c                   32.838(4)
_cell_measurement_reflns_used    74007
_cell_measurement_temperature    81(2)
_cell_measurement_theta_max      27.5204
_cell_measurement_theta_min      2.9999
_cell_volume                     25340(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      81(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            157529
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.63
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  0.8107
_exptl_absorpt_correction_T_min  0.6037
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             12726
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.177
_refine_diff_density_min         -2.203
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     5290
_refine_ls_number_reflns         88932
_refine_ls_number_restraints     4886
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1739
_reflns_number_gt                55585
_reflns_number_total             88932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408228b_si_002_2.cif
_cod_data_source_block           Compound-2
_cod_original_formula_sum        'C337 H655.50 Cu4 Mo48 N34.50 O164'
_cod_database_code               4121124