Polyoxometalatocyclophanes: Controlled Assembly of Polyoxometalate-Based Chiral Metallamacrocycles from Achiral Building Blocks
Fengping Xiao; Jian Hao; Jin Zhang; Chunlin Lv; Panchao Yin; Longsheng Wang; Yongge Wei; Journal of the American Chemical Society 132 (2010) 5956–5957; doi:10.1021/ja101671q

data_4102369
_publ_contact_author_address
;
Department of Chemistry
Tsinghua University
Beijing 100084
P. R. China
;
_publ_contact_author_email       yonggewei@mail.tsinghua.edu.cn
_publ_contact_author_name        'Dr Yongge Wei'
_publ_section_title
;
 Polyoxometalatocyclophanes: Controlled Assembly of Polyoxometalate-Based
 Chiral Metallamacrocycles from Achiral Building Blocks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5956
_journal_page_last               5957
_journal_paper_doi               10.1021/ja101671q
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C54 H99 Mo6 N5 O19'
_chemical_formula_weight         1698.02
_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                81.09(3)
_cell_angle_beta                 77.37(3)
_cell_angle_gamma                79.70(3)
_cell_formula_units_Z            2
_cell_length_a                   12.426(3)
_cell_length_b                   12.580(3)
_cell_length_c                   23.060(5)
_cell_measurement_reflns_used    20689
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      3.03
_cell_volume                     3435.5(15)
_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      296(2)
_diffrn_detector_area_resol_mean '100x100 micron'
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33972
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_T_max  0.8057
_exptl_absorpt_correction_T_min  0.6021
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         15180
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0732P)^2^+2.3742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1548
_reflns_number_gt                9989
_reflns_number_total             15180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja101671q_si_002_4.cif
_cod_data_source_block           3
_cod_original_cell_volume        3435.6(15)
_cod_database_code               4102369