Monopicolinate-dipicolyl Derivative of Triazacyclononane for Stable Complexation of Cu2+ and 64Cu2+
Melissa Roger; Luís M. P. Lima; Mathieu Frindel; Carlos Platas-Iglesias; Jean-François Gestin; Rita Delgado; Véronique Patinec; Raphaël Tripier; Inorganic Chemistry 52 (2013) 5246–5259; doi:10.1021/ic400174r

data_4334688
_publ_contact_author_address
;
Universite de Brest
UMR 6521 Laboratoire de chimie,
electrochimie moleculaire et chimie analytique 
6, avenue Victor Le Gorgeu
CS 93837
F-29238 BREST cedex 3
FRANCE
;
_publ_contact_author_email       raphael.tripier@univ-brest.fr
_publ_contact_author_name        'Tripier, Raphael'
_publ_section_title
;
 Monopicolinate-dipicolyl Derivative of Triazacyclononane for Stable
 Complexation of Cu2+ and 64Cu2+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5246
_journal_page_last               5259
_journal_paper_doi               10.1021/ic400174r
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
;
        C26 H32 Cu N6 O2 2+, (Cl O4 1-)2, H2 O
;
_chemical_formula_sum            'C26 H34 Cl2 Cu N6 O11'
_chemical_formula_weight         741.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_date             2012-05-31T17:14:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.901(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5089(2)
_cell_length_b                   22.8400(18)
_cell_length_c                   15.8525(3)
_cell_measurement_reflns_used    15292
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      31.5669
_cell_measurement_theta_min      2.8374
_cell_volume                     3080.4(3)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
        WinGX (Farrugia, 1999)
        PLATON (Spek, 1990-2003)
        enCIFer (Allen et al., 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1992)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0619185891
_diffrn_orient_matrix_UB_12      -0.0089808023
_diffrn_orient_matrix_UB_13      -0.0275230327
_diffrn_orient_matrix_UB_21      -0.015363925
_diffrn_orient_matrix_UB_22      0.0296619092
_diffrn_orient_matrix_UB_23      -0.0105503334
_diffrn_orient_matrix_UB_31      0.0536634506
_diffrn_orient_matrix_UB_32      -0.0019153156
_diffrn_orient_matrix_UB_33      -0.0336472093
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26979
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.84
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       'rounded prism, axis [1 0 0]'
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7636
_refine_ls_number_restraints     510
_refine_ls_restrained_S_all      1.334
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+4.5249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                6270
_reflns_number_total             7636
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400174r_si_002_1.cif
_cod_data_source_block           mr404-a
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4334688