Synthesis and structural characterization of BINOL-modified chiral polyoxometalates.
Ishimoto, Ryo; Kamata, Keigo; Suzuki, Kosuke; Yamaguchi, Kazuya; Mizuno, Noritaka; Dalton transactions (Cambridge, England : 2003) 44 (2015) 10947–10951; doi:10.1039/c5dt01338k

data_7035149
_publ_section_title
;
 Synthesis and structural characterization of BINOL-modified chiral
 polyoxometalates.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10947
_journal_page_last               10951
_journal_paper_doi               10.1039/c5dt01338k
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration S
_chemical_formula_sum            'C93 H181 N9 O51 Si Ti2 W10'
_chemical_formula_weight         4203.84
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-04-28 deposited with the CCDC.
2015-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0149(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8610(2)
_cell_length_b                   19.7487(2)
_cell_length_c                   36.5801(4)
_cell_measurement_temperature    113(2)
_cell_volume                     12903.0(2)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.959
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.959
_diffrn_reflns_point_group_measured_fraction_full 0.893
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.505
_diffrn_reflns_theta_min         0.557
_exptl_absorpt_coefficient_mu    9.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             8032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.636
_refine_diff_density_min         -2.899
_refine_diff_density_rms         0.352
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.002(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2992
_refine_ls_number_reflns         59263
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1044P)^2^+194.0275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.671
_reflns_friedel_fraction_full    0.788
_reflns_friedel_fraction_max     0.680
_reflns_number_gt                54350
_reflns_number_total             59263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01338k2.cif
_cod_data_source_block           S
_cod_depositor_comments
'Adding full bibliography for 7035148--7035149.cif.'
_cod_database_code               7035149
_shelxl_version_number           2013-3
_shelx_res_checksum              30670