Large (H2O)56(OH)6and (H2O)20Clusters inside a Nanometer-Sized M6L8Cage Constructed by Five-Coordinated Copper(II) and Flexible Carboxamide-Containing Tripodal Ligand
Wang, Yan; Okamura, Taka-aki; Sun, Wei-Yin; Ueyama, Norikazu; Crystal Growth & Design 8 (2008) 802–; doi:10.1021/cg701242z

data_4503521
_publ_section_title
;
 Large (H2O)56(OH)6and (H2O)20Clusters inside a Nanometer-Sized M6L8Cage
 Constructed by Five-Coordinated Copper(II) and Flexible
 Carboxamide-Containing Tripodal Ligand
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              802
_journal_paper_doi               10.1021/cg701242z
_journal_volume                  8
_journal_year                    2008
_chemical_formula_moiety         'C216 H515 B3 Cu6 F12 N48 O118 '
_chemical_formula_sum            'C216 H515 B3 Cu6 F12 N48 O118'
_chemical_formula_weight         6315.43
_chemical_name_systematic
; 
[Cu6(OH)6(TPMBA-4)8](BF4)3(OH)3-85(H2O) 
;
_space_group_IT_number           211
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      211
_symmetry_space_group_name_Hall  'I 4 2 3'
_symmetry_space_group_name_H-M   'I 4 3 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Wed May 17 17:40:10 2006'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   28.239(19)
_cell_length_b                   28.239(19)
_cell_length_c                   28.239(19)
_cell_measurement_reflns_used    1511
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     22519(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1549
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            84981
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6776
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.701
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.670
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3321
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.685
_refine_ls_R_factor_all          0.1812
_refine_ls_R_factor_gt           0.1573
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4066
_refine_ls_wR_factor_ref         0.4236
_reflns_number_gt                2474
_reflns_number_total             3321
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cg701242z-file002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        22518(27)
_cod_database_code               4503521