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_7030618
_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         'C26 H28 Cu3 N8 3+, 3(B F4 -)'
_chemical_formula_sum            'C26 H28 B3 Cu3 F12 N8'
_chemical_formula_weight         903.61
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 111.645(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.6904(8)
_cell_length_b                   23.414(2)
_cell_length_c                   8.8729(9)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.0
_cell_volume                     1678.1(3)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_publication_material  'teXsan Ver. 2.0'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_sigmaI/netI    0.1001
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11828
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.984
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.957
_refine_diff_density_min         -1.397
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3847
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.526
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0880
_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^)+(0.0982P)^2^+2.8758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2434
_reflns_number_gt                2845
_reflns_number_total             3847
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7000323
_cod_data_source_file            b812337c.txt
_cod_data_source_block           '[Cu3(pprd)2(AN)2(C2H4)2](BF4)3'
_cod_original_sg_symbol_Hall     '-P 2yb '
_cod_original_sg_symbol_H-M      'P 21/m '
_cod_original_formula_sum        'C26 H28 B3 Cu3 F12 N8 '
_cod_database_code               7030618