Copper(II) complexes of the isomeric tetraazamacrocyclic ligands 1,11- and 1,8-bis(2-pyridylmethyl)-1,4,8,11-tetraazacyclotetradecane and of the 1,4,8,11-tetraazacyclotetradecane-5,12-dione analogue at neutral and basic pH
Goeta, Andrés E.; Howard, Judith A. K.; Maffeo, Davide; Puschmann, Horst; Williams, J. A. Gareth; Yufit, Dimitrii S.; Journal of the Chemical Society, Dalton Transactions  (2000) 1873–; doi:10.1039/b000739k

data_7009407
_publ_section_title
;
 Copper(II) complexes of the isomeric tetraazamacrocyclic ligands 1,11-
 and 1,8-bis(2-pyridylmethyl)-1,4,8,11-tetraazacyclotetradecane and of
 the 1,4,8,11-tetraazacyclotetradecane-5,12-dione analogue at neutral
 and basic pH
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1873
_journal_paper_doi               10.1039/b000739k
_journal_year                    2000
_chemical_formula_sum            'C22 H32 Cu N6 O4'
_chemical_formula_weight         508.08
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.602(1)
_cell_angle_beta                 81.966(1)
_cell_angle_gamma                75.804(1)
_cell_formula_units_Z            2
_cell_length_a                   9.7924(3)
_cell_length_b                   10.3659(3)
_cell_length_c                   12.6077(3)
_cell_measurement_reflns_used    6089
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      2.7
_cell_volume                     1137.37(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11566
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.002
_exptl_absorpt_correction_T_max  0.9064
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            clear-purple
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.344
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5888
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.344
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.258
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.2158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                4674
_reflns_number_total             5888
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b000739k.txt
_cod_data_source_block           CuL3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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_sg_symbol_H-M      P-1
_cod_database_code               7009407