Spontaneous Resolution of Evans-Showell-Type Polyoxometalates in Constructing Chiral Inorganic-Organic Hybrid Architectures.
An, Haiyan; Wang, Lin; Hu, Ying; Xu, Tieqi; Hou, Yujiao; Inorganic chemistry 55 (2016) 144–153; doi:10.1021/acs.inorgchem.5b01994

data_4346710
_publ_section_title
;
 Spontaneous Resolution of Evans-Showell-Type Polyoxometalates in
 Constructing Chiral Inorganic-Organic Hybrid Architectures.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              144
_journal_page_last               153
_journal_paper_doi               10.1021/acs.inorgchem.5b01994
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C32 H58 Co2 Mo10 N4 Ni O57'
_chemical_formula_weight         2546.79
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                103.364(5)
_cell_angle_beta                 94.848(6)
_cell_angle_gamma                104.852(5)
_cell_formula_units_Z            1
_cell_length_a                   9.9724(9)
_cell_length_b                   13.5235(14)
_cell_length_c                   13.5824(15)
_cell_measurement_reflns_used    10289
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      1.559
_cell_volume                     1702.4(3)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10289
_diffrn_reflns_point_group_measured_fraction_full 0.557
_diffrn_reflns_point_group_measured_fraction_max 0.573
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.559
_exptl_absorpt_coefficient_mu    2.639
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.484
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.004(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         6857
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.9952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0623
_reflns_Friedel_coverage         0.152
_reflns_Friedel_fraction_full    0.147
_reflns_Friedel_fraction_max     0.152
_reflns_number_gt                6665
_reflns_number_total             6857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01994_si_002.cif
_cod_data_source_block           3
_cod_database_code               4346710
_shelxl_version_number           2014-3
_shelx_res_checksum              30850
_shelx_hkl_checksum              15824