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_4121123
_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            'C39 H75 Mo6 N3 O20'
_chemical_formula_weight         1481.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.685(4)
_cell_length_b                   15.242(3)
_cell_length_c                   20.150(4)
_cell_measurement_reflns_used    1826
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.76
_cell_measurement_theta_min      3.03
_cell_volume                     5225(2)
_computing_cell_refinement       'Rigaku RAPID AUTO Ver2.30'
_computing_data_collection       'Rigaku RAPID AUTO Ver2.30'
_computing_data_reduction        'Rigaku RAPID AUTO Ver2.30'
_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      293(2)
_diffrn_detector_area_resol_mean '100x100 micron'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42209
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  0.5908
_exptl_absorpt_correction_T_min  0.5268
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_description       block
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.950
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         10225
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.1599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                8043
_reflns_number_total             10225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408228b_si_002_1.cif
_cod_data_source_block           Compound-1
_cod_original_cell_volume        5224.7(20)
_cod_database_code               4121123