Thermodynamic and structural properties of Gd3+ complexes with functionalized macrocyclic ligands based upon 1,4,7,10-tetraazacyclododecane
Bianchi, Antonio; Calabi, Luisella; Giorgi, Claudia; Losi, Pietro; Mariani, Palma; Paoli, Paola; Rossi, Patrizia; Valtancoli, Barbara; Virtuani, Mario; Journal of the Chemical Society, Dalton Transactions  (2000) 697–; doi:10.1039/a909098c

data_7009173
_publ_section_title
;
 Thermodynamic and structural properties of Gd3+ complexes with
 functionalized macrocyclic ligands based upon
 1,4,7,10-tetraazacyclododecane
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              697
_journal_paper_doi               10.1039/a909098c
_journal_year                    2000
_chemical_formula_moiety
;
Gd 3+, C20 H40 N8 O4, Na +, (Cl O4 1-)4, (H2 O)4
;
_chemical_formula_structural
;
(Gd (H2 O) (C20 H40 N8 O4)) (Cl O4)3 (Na) (Cl O4) (H2 O)3
;
_chemical_formula_sum            'C20 H48 Cl4 Gd N8 Na O24'
_chemical_formula_weight         1106.70
_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
_cell_angle_alpha                94.29(9)
_cell_angle_beta                 109.65(8)
_cell_angle_gamma                102.97(6)
_cell_formula_units_Z            2
_cell_length_a                   11.558(6)
_cell_length_b                   13.251(9)
_cell_length_c                   14.713(9)
_cell_measurement_temperature    298
_cell_volume                     2040(3)
_computing_cell_refinement       'CAD4 Enraf Nonius'
_computing_data_collection       'CAD4 Enraf Nonius'
_computing_data_reduction        'CAD4 Enraf Nonius'
_computing_molecular_graphics    'Ortep (Johnson, 1971)'
_computing_publication_material  'Parst93 (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'Sir92 (Altomare et al.)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'ENRAF NONIUS CAD4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7410
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.993
_exptl_absorpt_correction_type   'refdelf (Walker and Stuart, 1983)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.391
_refine_diff_density_min         -2.008
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         7111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_obs          0.0496
_refine_ls_shift/esd_max         0.234
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+4.7667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1390
_refine_ls_wR_factor_obs         0.1306
_reflns_number_observed          6377
_reflns_number_total             7114
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a909098c.txt
_cod_data_source_block           '[Gd(DTMA)H2O](ClO4)3'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+4.7667P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+4.7667P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2040.1(21)
_cod_database_code               7009173