Synthetic, Structural, Spectroscopic, Electrochemical Studies and Self-assembly of Nanoscale Polyoxometalate−Organic Hybrid Molecular Dumbbells
Zhu, Yi; Wang, Longsheng; Hao, Jian; Xiao, Zicheng; Wei, Yongge; Wang, Yuan; Crystal Growth & Design 9 (2009) 3509–; doi:10.1021/cg9002516

data_4511134
_publ_section_title
;
 Synthetic, Structural, Spectroscopic, Electrochemical Studies and
 Self-assembly of Nanoscale Polyoxometalate&#x2212;Organic Hybrid
 Molecular Dumbbells
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3509
_journal_paper_doi               10.1021/cg9002516
_journal_volume                  9
_journal_year                    2009
_chemical_formula_sum            'C76 H153 Mo12 N6 O36.5'
_chemical_formula_weight         2886.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.53(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.109(5)
_cell_length_b                   25.207(5)
_cell_length_c                   19.314(4)
_cell_measurement_reflns_used    41712
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      3
_cell_volume                     11198(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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0888
_diffrn_reflns_av_sigmaI/netI    0.0899
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            73949
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.367
_exptl_absorpt_correction_T_max  0.9348
_exptl_absorpt_correction_T_min  0.6845
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             5788
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1181
_refine_ls_number_reflns         17226
_refine_ls_number_restraints     748
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0018P)^2^+98.9889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1605
_reflns_number_gt                10138
_reflns_number_total             17226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg9002516_si_001.cif
_cod_data_source_block           Compound_2
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_original_formula_sum        'C76 H153 Mo12 N6 O36.50'
_cod_database_code               4511134