Ternary complexes composed of naphthalene diimides and binucleating metallocavitands: preparation, characterisation and structure of [(Ni2L)2(NDI)][BPh4]2
Lee, Katrina A.; Lozan, Vasile; Langford, Steven J.; Kersting, Berthold; Dalton Transactions  (2009) 7481–7485; doi:10.1039/b907785e

data_7002178
_publ_section_title
;
 Ternary complexes composed of naphthalene diimides and binucleating
 metallocavitands: preparation, characterisation and structure of
 [(Ni2L)2(NDI)][BPh4]2
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              7481
_journal_page_last               7485
_journal_paper_doi               10.1039/b907785e
_journal_year                    2009
_chemical_compound_source
;
Crystals were grown by recrystallization from acetonitrile
;
_chemical_formula_moiety         'C96 H140 N14 Ni4 O8 S4, B2 C48 H40, C4 H6 N2'
_chemical_formula_structural
;
[(Ni2L)2(NDI-dicarboxylate)](BPh4)2(MeCN)x
;
_chemical_formula_sum            'C148 H186 B2 N16 Ni4 O8 S4'
_chemical_formula_weight         2701.83
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                100.928(7)
_cell_angle_beta                 109.095(6)
_cell_angle_gamma                94.584(7)
_cell_formula_units_Z            1
_cell_length_a                   14.0287(11)
_cell_length_b                   16.6371(16)
_cell_length_c                   18.5087(16)
_cell_measurement_reflns_used    17802
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      51.16
_cell_measurement_theta_min      3.85
_cell_volume                     3961.0(6)
_computing_cell_refinement       'STOE X-Area'
_computing_data_collection       'STOE X-Area'
_computing_data_reduction        'STOE X-Area'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       hemisphere
_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  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27135
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.8935
_exptl_absorpt_correction_T_min  0.8462
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         13686
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0786P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1404
_reflns_number_gt                8686
_reflns_number_total             13686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907785e.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7002178