A unique chair-shaped hexanuclear Cu(I) metallamacrocyclic C2H4 adduct encapsulating a BF4− anion
Maekawa, Masahiko; Nabei, Atsuhiro; Tominaga, Toshi; Sugimoto, Kunihisa; Minematsu, Toshie; Okubo, Takashi; Kuroda-Sowa, Takayoshi; Munakata, Megumu; Kitagawa, Susumu; Dalton Transactions  (2009) 415–417; doi:10.1039/b812337c

data_7000324
_publ_section_title
;
 A unique chair-shaped hexanuclear Cu(I) metallamacrocyclic C2H4 adduct
 encapsulating a BF4&#x2212; anion
;
_journal_coden_ASTM              DTARAF
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              415
_journal_page_last               417
_journal_paper_doi               10.1039/b812337c
_journal_year                    2009
_chemical_formula_moiety         'C66 H72 B6 Cu6 F24 N18 O3 '
_chemical_formula_sum            'C66 H72 B6 Cu6 F24 N18 O3'
_chemical_formula_weight         2067.52
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   27.6972(15)
_cell_length_b                   27.6972(15)
_cell_length_c                   19.8549(16)
_cell_measurement_reflns_used    7840
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     13190.8(15)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        CRYSTALCLEAR
_computing_publication_material  'Crystal Structure 3.8'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33514
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  0.8260
_exptl_absorpt_correction_T_min  0.6570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             6228
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.091
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.895
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6725
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.917
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.1063
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3126
_refine_ls_wR_factor_ref         0.3483
_reflns_number_gt                4036
_reflns_number_total             6725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B812337C.txt
_cod_data_source_block           {[Cu6(pprd)6(C2H4)6](BF4)6}2.6H2O
_cod_original_sg_symbol_Hall     '-R 3 '
_cod_original_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        'C66 H72 B6 Cu6 F24 N18 O3 '
_cod_database_code               7000324