Lanthanide(III) Complexes with a Tetrapyridine Pendant-Armed Macrocyclic Ligand: 1H NMR Structural Determination in Solution, X-ray Diffraction, and Density-Functional Theory Calculations
del C. Fernández-Fernández, M.; Bastida, R.; Macías, A.; Pérez-Lourido, P.; Platas-Iglesias, C.; Valencia, L.; Inorganic Chemistry 45 (2006) 4484–4496; doi:10.1021/ic0603508

data_4332421
_publ_section_title
;
 Lanthanide(III) Complexes with a Tetrapyridine Pendant-Armed Macrocyclic
 Ligand:&#x00A0;1H NMR Structural Determination in Solution, X-ray
 Diffraction, and Density-Functional Theory Calculations
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4484
_journal_page_last               4496
_journal_paper_doi               10.1021/ic0603508
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C42 H46 Gd2 N16 O22'
_chemical_formula_weight         1441.45
_chemical_name_systematic
;
 ?
;
_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                 92.8780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2551(8)
_cell_length_b                   20.9320(12)
_cell_length_c                   17.6226(10)
_cell_measurement_temperature    293(2)
_cell_volume                     5251.7(5)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_computing_data_reduction        'BRUKER Shelxtl'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXLS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  Smart-CCD-1000
_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  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0901
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34561
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    2.600
_exptl_absorpt_correction_T_max  0.6811
_exptl_absorpt_correction_T_min  0.4545
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.766
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         12398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                7823
_reflns_number_total             12398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0603508sup1.cif
_cod_data_source_block           '[Gd(L)][Gd(NO3)4(H20)2].2NO3.2H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4332421