Oxo-anion recognition by mono- and bisurea pendant-arm macrocyclic complexes.
Boiocchi, Massimo; Licchelli, Maurizio; Milani, Michele; Poggi, Antonio; Sacchi, Donatella; Inorganic chemistry 54 (2015) 47–58; doi:10.1021/ic501527k

data_4341985
_publ_contact_author
;
  Maurizio Licchelli
  Dipartimento di Chimica Generale
  University of Pavia
  via Taramelli 12, I-27100 Pavia, ITALY
;
_publ_section_title
;
 Oxo-anion recognition by mono- and bisurea pendant-arm macrocyclic
 complexes.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              47
_journal_page_last               58
_journal_paper_doi               10.1021/ic501527k
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C26 H40 Cu N12 O6, 6(C2 H6 O S), 2(Cl O4)'
_chemical_formula_sum            'C38 H76 Cl2 Cu N12 O20 S6'
_chemical_formula_weight         1347.98
_chemical_name_common
;
(3,10-bis(2-(3-(4-nitrophenyl)urea)ethyl)-1,3,5,8,10,12-hexa-
azacyclotetradecane)-copper(ii) diperchlorate dimethyl sulfoxide hexa-solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.14(2)
_cell_angle_beta                 74.18(2)
_cell_angle_gamma                70.85(2)
_cell_formula_units_Z            1
_cell_length_a                   10.259(3)
_cell_length_b                   12.451(3)
_cell_length_c                   14.554(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     1584.9(8)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega scans'
_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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7859
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        35
_diffrn_standards_interval_time  300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.6790
_exptl_absorpt_correction_T_min  0.6261
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
;
_exptl_crystal_colour            'PALE RED'
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             707
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         5553
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+1.0234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1933
_reflns_number_gt                3490
_reflns_number_total             5553
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic501527k_si_002.cif
_cod_data_source_block           '[3]_ClO4_DMSO'
_cod_depositor_comments
'Adding full bibliography for 4341984--4341986.cif.'
_cod_database_code               4341985
_diffrn_standards_corr_method    'STDANAL linear fit'