Nanoscale chiral rod-like molecular triads assembled from achiral polyoxometalates.
Zhang, Jin; Hao, Jian; Wei, Yongge; Xiao, Fengping; Yin, Panchao; Wang, Longsheng; Journal of the American Chemical Society 132 (2010) 14–15; doi:10.1021/ja907535g

data_4101632
_publ_section_title
;
 Nanoscale chiral rod-like molecular triads assembled from achiral
 polyoxometalates.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14
_journal_page_last               15
_journal_paper_doi               10.1021/ja907535g
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C62 H135 Mn0.5 Mo9 N5.5 O30'
_chemical_formula_weight         2328.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.174(3)
_cell_length_b                   18.174(3)
_cell_length_c                   49.125(10)
_cell_measurement_reflns_used    60568
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.10
_cell_volume                     14052(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0767
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            98862
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  0.5631
_exptl_absorpt_correction_T_min  0.4233
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7056
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_coef       0.00085(6)
_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   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         18345
_refine_ls_number_restraints     554
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+22.6759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                12564
_reflns_number_total             18345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja907535g_si_003.cif
_cod_data_source_block           zj
_cod_original_cell_volume        14051(4)
_cod_original_formula_sum        'C62 H135 Mn0.50 Mo9 N5.50 O30'
_cod_database_code               4101632