A new dipyridine-containing cryptand for both proton and Cu(ii) encapsulation. A solution and solid state study
Bazzicalupi, Carla; Bellusci, Anna; Bencini, Andrea; Berni, Emanuela; Bianchi, Antonio; Ciattini, Samuele; Giorgi, Claudia; Valtancoli, Barbara; Journal of the Chemical Society, Dalton Transactions  (2002) 2151–; doi:10.1039/b200486k

data_7011487
_publ_section_title
;
 A new dipyridine-containing cryptand for both proton and Cu(ii)
 encapsulation. A solution and solid state study
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2151
_journal_paper_doi               10.1039/b200486k
_journal_year                    2002
_chemical_formula_moiety
;
(C17 H23 N5 Cu 2+), (Cl O4 1-)2
;
_chemical_formula_sum            'C17 H23 Cl2 Cu N5 O8'
_chemical_formula_weight         559.84
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.973(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1570(10)
_cell_length_b                   8.8210(10)
_cell_length_c                   20.685(3)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    298
_cell_measurement_theta_max      42
_cell_measurement_theta_min      12
_cell_volume                     2177.6(4)
_computing_cell_refinement       XSCANS-Bruker
_computing_data_collection       XSCANS-Bruker
_computing_data_reduction        XSCANS-Bruker
_computing_molecular_graphics    'ORTEP-3 (Ver. 1.01\b) (Farrugia, 1997)'
_computing_publication_material  'Parst97 (Nardelli, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'SIEMENS P4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4100
_diffrn_reflns_theta_full        59.99
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.186
_exptl_absorpt_correction_T_max  0.42
_exptl_absorpt_correction_T_min  0.27
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   PSI-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0058(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         3034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0684
_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^)+(0.1214P)^2^+4.0446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1885
_refine_ls_wR_factor_ref         0.2012
_reflns_number_gt                2568
_reflns_number_total             3034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200486k.txt
_cod_data_source_block           '[CuL1](ClO4)2'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7011487
_atom_sites_solution_h1n3        geom
_refine_ls_h1n3_treatment        refall
_atom_sites_solution_h1n5        geom
_refine_ls_h1n5_treatment        refall