Monopicolinate Cross-Bridged Cyclam Combining Very Fast Complexation with Very High Stability and Inertness of Its Copper(II) Complex.
Lima, Luís M P; Halime, Zakaria; Marion, Ronan; Camus, Nathalie; Delgado, Rita; Platas-Iglesias, Carlos; Tripier, Raphaël; Inorganic chemistry 53 (2014) 5269–5279; doi:10.1021/ic500491c

data_4338203
_publ_section_title
;
 Monopicolinate Cross-Bridged Cyclam Combining Very Fast Complexation with
 Very High Stability and Inertness of Its Copper(II) Complex.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5269
_journal_page_last               5279
_journal_paper_doi               10.1021/ic500491c
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety
;
C19 H33 N5 O2 2+, (Cl O4 -)2
;
_chemical_formula_sum            'C19 H33 Cl2 N5 O10'
_chemical_formula_weight         562.4
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-09-13T15:37:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.561(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1484(9)
_cell_length_b                   14.8319(12)
_cell_length_c                   14.8211(11)
_cell_measurement_reflns_used    2674
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      31.7831
_cell_measurement_theta_min      3.0923
_cell_volume                     2423.4(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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0452186065
_diffrn_orient_matrix_UB_12      0.03177267
_diffrn_orient_matrix_UB_13      -0.0173392313
_diffrn_orient_matrix_UB_21      0.0443184859
_diffrn_orient_matrix_UB_22      0.0260047557
_diffrn_orient_matrix_UB_23      -0.0179970671
_diffrn_orient_matrix_UB_31      -0.0115284069
_diffrn_orient_matrix_UB_32      -0.0245202973
_diffrn_orient_matrix_UB_33      -0.0414326454
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.1071
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9238
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.39
_exptl_absorpt_coefficient_mu    0.333
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.938
_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            colourless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             1184
_exptl_crystal_recrystallization_method
;
slow evaporation of aqueous solution at room temperature
;
_exptl_crystal_size_max          0.3117
_exptl_crystal_size_mid          0.2036
_exptl_crystal_size_min          0.0613
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.61
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881
1571 Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.07(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4053
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0637P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                2501
_reflns_number_total             4053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500491c_si_002.cif
_cod_data_source_block           rm1-72co-a0
_cod_depositor_comments          'Adding full bibliography for 4338203.cif.'
_cod_original_sg_symbol_Hall     C-2yc
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4338203