Monopicolinate Cyclen and Cyclam Derivatives for Stable Copper(II) Complexation
Luís M. P. Lima; David Esteban-Gómez; Rita Delgado; Carlos Platas-Iglesias; Raphaël Tripier; Inorganic Chemistry 51 (2012) 6916–6927; doi:10.1021/ic300784v

data_4329549
_publ_contact_author_address
;
Laboratoire de chimie,
electrochimie moleculaire et chimie analytique (UMR 6521)
Universite de Bretagne occidentale
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 Cyclen and Cyclam Derivatives for Stable Copper(II)
 Complexation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6916
_journal_page_last               6927
_journal_paper_doi               10.1021/ic300784v
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
;
        C15 H25 Cu N5 O2 2+, (Cl O4 -)2, H2 O
;
_chemical_formula_sum            'C15 H27 Cl2 Cu N5 O11'
_chemical_formula_weight         587.86
_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             2011-07-29T19:55:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.399(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8699(5)
_cell_length_b                   11.6792(5)
_cell_length_c                   16.8272(7)
_cell_measurement_reflns_used    4192
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      31.6233
_cell_measurement_theta_min      2.9719
_cell_volume                     2332.71(17)
_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  'PLATON (Spek, 1980-2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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      0.0587140152
_diffrn_orient_matrix_UB_12      0.0029832582
_diffrn_orient_matrix_UB_13      -0.007177406
_diffrn_orient_matrix_UB_21      -0.0076670484
_diffrn_orient_matrix_UB_22      0.0530911052
_diffrn_orient_matrix_UB_23      -0.0197904251
_diffrn_orient_matrix_UB_31      0.0078343458
_diffrn_orient_matrix_UB_32      0.0293152797
_diffrn_orient_matrix_UB_33      0.0365215629
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0856
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17589
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.231
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.830
_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    1.674
_exptl_crystal_description
;
        fragment of flat hexagon // (1 0 0)
;
_exptl_crystal_F_000             1212
_exptl_crystal_recrystallization_method
;
slow evaporation of aqueous solution at room temperature
;
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4765
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0667
_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^)+(0.1083P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.1874
_reflns_number_gt                2780
_reflns_number_total             4765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300784v_si_002_4.cif
_cod_data_source_block           aa08cu-a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4329549