A new class of macrocycle capable of binding exogenous metals: synthesis, structure, magnetic and electrochemical properties of a Cu(II) trinuclear complex based upon 1,4,8,11-tetraazacyclotetradecane-2,3-dione [exoO2]cyclam †
Cronin, Leroy; Mount, Andrew R.; Parsons, Simon; Robertson, Neil; Journal of the Chemical Society, Dalton Transactions  (1999) 1925–; doi:10.1039/a902792k

data_7027443
_publ_section_title
;
 A new class of macrocycle capable of binding exogenous metals: synthesis,
 structure, magnetic and electrochemical properties of a Cu(II) trinuclear
 complex based upon 1,4,8,11-tetraazacyclotetradecane-2,3-dione
 [exoO2]cyclam&#x200A;&#x2020;
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_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1925
_journal_paper_doi               10.1039/a902792k
_journal_year                    1999
_chemical_formula_moiety         '2 (Cl O4) C20 H44 Cu3 N8 O6'
_chemical_formula_sum            'C20 H44 Cl2 Cu3 N8 O16'
_chemical_formula_weight         914.16
_chemical_name_common            {Cu[exoO~2~cyclam]}~2~Cu(ClO4)~2~2H~2~O
_chemical_name_systematic
;[((1,4,8,11-tetraaza-\k^4^N)-cyclotetradecane-2,3-
dione-(hydrato-/kO)copper(II))2-\k^4^O-copper(II))]
bis perchlorate dihydrate
;
_chemical_temperature_decomposition_gt 160
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 106.208(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.6599(17)
_cell_length_b                   16.907(4)
_cell_length_c                   12.784(2)
_cell_measurement_reflns_used    56
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      66
_cell_measurement_theta_min      60
_cell_volume                     1797.3(6)
_computing_molecular_graphics    'WINGX PACKAGE (L. J. Farrugia, 1998)'
_computing_publication_material  'WINGX PACKAGE (L. J. Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (A. Guagliardi, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Stoe Stadi-4B'
_diffrn_measurement_method       \w\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3746
_diffrn_reflns_theta_full        70.07
_diffrn_reflns_theta_max         70.07
_diffrn_reflns_theta_min         4.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.113
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       'none refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3171
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0987P)^2^+0.9945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1532
_reflns_number_gt                2553
_reflns_number_total             3171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            902792ksup1.cif
_cod_data_source_block           lc112f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition_gt' since the value was
specified 'more than' ('>') a certain temperature. The value '>160
(dec.)' was changed to '160' - it should be numeric and without a
unit designator.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1797.4(6)
_cod_original_sg_symbol_H-M      'P 21 / n'
_cod_database_code               7027443