Supramolecular self-assembly for designing non-centrosymmetric crystals based on Keggin polyoxometallates and crown ether.
Xiong, Jun; Kubo, Kazuya; Lü, Shao-Fang; Li, Ming; Nakamura, Takayoshi; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14001–14007; doi:10.1039/c8dt02910e

data_7701905
_publ_section_title
;
 Supramolecular self-assembly for designing non-centrosymmetric crystals
 based on Keggin polyoxometallates and crown ether.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14001
_journal_page_last               14007
_journal_paper_doi               10.1039/c8dt02910e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C56 H68 Br2 Mo12 N4 O52 S'
_chemical_formula_weight         2972.28
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-11-27 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.465(2)
_cell_length_b                   24.416(5)
_cell_length_c                   17.474(4)
_cell_measurement_reflns_used    1
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.005
_cell_measurement_theta_min      3.005
_cell_volume                     4325.3(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39745
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    2.728
_exptl_absorpt_correction_type   Rigaku
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3565
_refine_diff_density_max         1.672
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         9839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+8.0288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                8486
_reflns_number_total             9839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt02910e2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        4325.1(15)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               7701905