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_7030617
_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         'C13 H15 Cu2 N5 O6 '
_chemical_formula_sum            'C13 H15 Cu2 N5 O6'
_chemical_formula_weight         464.38
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.603(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7587(11)
_cell_length_b                   8.1512(6)
_cell_length_c                   15.7527(13)
_cell_measurement_reflns_used    3689
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1724.1(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_sigmaI/netI    0.0998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22732
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         31.70
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    2.508
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5351
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1511
_refine_ls_R_factor_gt           0.0767
_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^)+(0.0255P)^2^+5.3342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                3065
_reflns_number_total             5351
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7000322
_cod_data_source_file            b812337c.txt
_cod_data_source_block           '[Cu2(pprd)(C2H4)2(NO3)]NO3'
_cod_original_formula_sum        'C13 H15 Cu2 N5 O6 '
_cod_database_code               7030617