New Bis-Cresol-Bridged bis(1,4,7-Triazacyclononane) Ligand As Receptor for Metal Cations and Phosphate Anions
Enrico Arturoni; Carla Bazzicalupi; Andrea Bencini; Claudia Caltagirone; Andrea Danesi; Alessandra Garau; Claudia Giorgi; Vito Lippolis; Barbara Valtancoli; Inorganic Chemistry 47 (2008) 6551–6563; doi:10.1021/ic800549e

data_4305566
_publ_contact_author_address
;  Department of Chemistry
   University of Florence
   Via della Lastruccia 3
   50019 Sesto Fiorentino
   Florence
   Italy
;
_publ_contact_author_email       andrea.bencini@unifi.it
_publ_contact_author_fax         39(055)4573364
_publ_contact_author_phone       39(055)4573371
_publ_section_title
;
New Bis-Cresol-Bridged bis(1,4,7-Triazacyclononane) Ligand As Receptor for
Metal Cations and Phosphate Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6551
_journal_page_last               6563
_journal_paper_doi               10.1021/ic800549e
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C29 H48 Cu2 N8 O10'
_chemical_formula_weight         795.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.05230(10)
_cell_length_b                   28.3800(4)
_cell_length_c                   16.1372(2)
_cell_measurement_reflns_used    9788
_cell_measurement_temperature    298
_cell_measurement_theta_max      72.1834
_cell_measurement_theta_min      4.1469
_cell_volume                     3687.74(8)
_computing_cell_refinement       'Crysalis CCD - Oxford diffraction'
_computing_data_collection       'Crysalis CCD - Oxford diffraction'
_computing_data_reduction        'Crysalis CCD - Oxford diffraction'
_computing_molecular_graphics
;
ORTEP3 Ver. 1.01\b (Farrugia, 1997) - Mercury 2001-2007
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla 2005)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 8.1241
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur CCD'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24113
_diffrn_reflns_theta_full        72.32
_diffrn_reflns_theta_max         72.32
_diffrn_reflns_theta_min         5.42
_diffrn_standards_interval_count infinity
_diffrn_standards_interval_time  infinity
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.953
_exptl_absorpt_correction_T_max  0.677
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.2 (release 07-07-2006 CrysAlis171 .NET)
(compiled Jul 10 2006,00:11:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.263
_refine_diff_density_min         -1.374
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.363
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3606
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.381
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0677
_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^)+(0.1278P)^2^+0.9021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2081
_refine_ls_wR_factor_ref         0.2358
_reflns_number_gt                2682
_reflns_number_total             3606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800549e-file005.cif
_cod_data_source_block           '[Cu2L(NO3)2].2H2O'
_cod_database_code               4305566