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_7047462
_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_moiety         'C174 H168 Cu6 La2 N12 O12, C7 H8'
_chemical_formula_sum            'C181 H176 Cu6 La2 N12 O12'
_chemical_formula_weight         3370.39
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-21 deposited with the CCDC.
2018-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.22(3)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   15.565(13)
_cell_length_b                   11.095(8)
_cell_length_c                   23.637(13)
_cell_measurement_reflns_used    9707
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.461
_cell_measurement_theta_min      3.140
_cell_volume                     3919(5)
_computing_data_collection       'Bruker APEX3 v2016.1-0'
_computing_data_reduction        'SAINT V8.38A (2016)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'CMOS area detector'
_diffrn_measurement_device_type  'Bruker D8QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.1378
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            138412
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         3.099
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2016/2'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       plank
_exptl_crystal_F_000             1730
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.937
_refine_diff_density_min         -1.656
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1088
_refine_ls_number_reflns         17923
_refine_ls_number_restraints     712
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0692
_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^)+(0.0799P)^2^+12.6118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1763
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                13418
_reflns_number_total             17923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02910e2.cif
_cod_data_source_block           40244
_cod_depositor_comments
'Adding full bibliography for 7047460--7047465.cif.'
_cod_database_code               7047462
_shelx_shelxl_version_number     2017/1