Self-assembly hexanuclear metallacontainer hosting halogenated guest species and sustaining structure of 3D coordination framework
Evgen Govor; Andrey Lysenko; David Quinonero; Eduard Rusanov; Alexander Chernega; Jens Moellmer; Reiner Staudt; Harald Krautscheid; Antonio Frontera; Konstantin Domasevitch; Chem.Commun. 47 (2011) 1764–; doi:10.1039/c0cc04433d

data_7105932
_publ_section_title
;
 Self-assembly hexanuclear metallacontainer hosting halogenated guest
 species and sustaining structure of 3D coordination framework
;
_journal_name_full               Chem.Commun.
_journal_page_first              1764
_journal_paper_doi               10.1039/c0cc04433d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety
'C42 H54 Cl Cu6 N30 O6, C20 H40 K O10, 2(C4 H8 O2), 4(C H Cl3)'
_chemical_formula_sum            'C74 H114 Cl13 Cu6 K N30 O20'
_chemical_formula_weight         2625.14
_chemical_name_systematic
;
bis-(1,4-dioxane)-(1,4,7,10,13,16-hexaoxacyclooctadecane)potassium
\m6-chlorido-hexakis-[\m-(4-(1,2,4-triazol-4-yl)-3,5-dimethylpyrazolato]-
hexa-\m-hydroxido-hexacopper(II) Solvate with 4 Chloroform and 2
1,4-Dioxane
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.674(2)
_cell_angle_beta                 70.698(2)
_cell_angle_gamma                74.380(2)
_cell_formula_units_Z            1
_cell_length_a                   13.9372(5)
_cell_length_b                   14.5888(5)
_cell_length_c                   15.0259(6)
_cell_measurement_reflns_used    22499
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      5.52
_cell_volume                     2773.01(18)
_computing_cell_refinement       'SAINT-NT (Bruker, 1999)'
_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_data_reduction        'SAINT-NT (Bruker, 1999)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEXII area-detector diffractometer'
_diffrn_measurement_method       '\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  0.0602
_diffrn_reflns_av_sigmaI/netI    0.1154
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22499
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         5.52
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.554
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6444
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         10284
_refine_ls_number_restraints     280
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1761
_reflns_number_gt                5576
_reflns_number_total             10284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC04433D.TXT
_cod_data_source_block           (1)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7105932