Self-assembly of nanometre-scale metallacalix[4]arene building blocks and Keggin units to a novel (3,4)-connected 3D self-penetrating framework.
Wang, Xiuli; Hu, Hailiang; Liu, Guocheng; Lin, Hongyan; Tian, Aixiang; Chemical communications (Cambridge, England) 46 (2010) 6485–6487; doi:10.1039/c0cc01412e

data_7112805
_publ_section_title
;
 Self-assembly of nanometre-scale metallacalix[4]arene building blocks and
 Keggin units to a novel (3,4)-connected 3D self-penetrating framework.
;
_journal_issue                   35
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6485
_journal_page_last               6487
_journal_paper_doi               10.1039/c0cc01412e
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         '2(C63 H108 Cu12 N72 O160 S18 Si4 W48), O'
_chemical_formula_sum            'C126 H222 Cu24 N144 O321 S36 Si8 W96'
_chemical_formula_weight         29443.92
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   27.0553(15)
_cell_length_b                   27.0553(15)
_cell_length_c                   63.159(4)
_cell_measurement_reflns_used    9643
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      25.0358
_cell_measurement_theta_min      2.3877
_cell_volume                     40038(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -74
_diffrn_reflns_number            96467
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    21.777
_exptl_absorpt_correction_T_max  0.1111
_exptl_absorpt_correction_T_min  0.1039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' SADABS, Sheldrick, 1996'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             39126
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         3.486
_refine_diff_density_min         -2.322
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1177
_refine_ls_number_reflns         15667
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+1078.4564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                12215
_reflns_number_total             15667
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc01412e.txt
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7112805