Spontaneous resolution of a chiral polyoxometalate: Synthesis, crystal structures and properties
Cai, L; Li, Y; Yu, C; Ji, H; Liu, Y; Liu, S; Inorganica Chimica Acta 362 (2009) 2895–2899; doi:10.1016/j.ica.2009.01.013

data_1507779
_publ_section_title
;
 Spontaneous resolution of a chiral polyoxometalate: Synthesis, crystal
 structures and properties
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              2895
_journal_page_last               2899
_journal_paper_doi               10.1016/j.ica.2009.01.013
_journal_volume                  362
_journal_year                    2009
_chemical_formula_sum            'C20 H100 N10 O88 P2 W22 Zr'
_chemical_formula_weight         6086.67
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.4360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2742(9)
_cell_length_b                   20.5699(15)
_cell_length_c                   20.9526(15)
_cell_measurement_reflns_used    17915
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      0.97
_cell_volume                     5289.9(7)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       \w
_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  0.0801
_diffrn_reflns_av_sigmaI/netI    0.1250
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27002
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    24.013
_exptl_absorpt_correction_T_max  0.073
_exptl_absorpt_correction_T_min  0.047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.821
_exptl_crystal_density_meas      3.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular hexagonal prism'
_exptl_crystal_F_000             4752
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.223
_refine_diff_density_min         -4.280
_refine_diff_density_rms         0.580
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         17915
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0732
_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^)+(0.1044P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.1883
_reflns_number_gt                15007
_reflns_number_total             17915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            702813-R-1.cif
_cod_data_source_block           compound_R-1
_cod_original_sg_symbol_H-M      P21
_cod_original_formula_sum        'C20 H100 N10 O88 P2 W22 Zr '
_cod_database_code               1507779