Lanthanide(III) Complexes with Ligands Derived from a Cyclen Framework Containing Pyridinecarboxylate Pendants. The Effect of Steric Hindrance on the Hydration Number
Aurora Rodríguez-Rodríguez; David Esteban-Gómez; Andrés de Blas; Teresa Rodríguez-Blas; Marianna Fekete; Mauro Botta; Raphaël Tripier; Carlos Platas-Iglesias; Inorganic Chemistry 51 (2012) 2509–2521; doi:10.1021/ic202436j

data_4328417
_publ_contact_author_address
;
Departamento de Quimica Fundamental
Facultade de Ciencias
Universidade da Coru\~na
Rua da Fraga 10
15008 A Coru\~na
Spain
;
_publ_contact_author_email       andres.blas@udc.es
_publ_contact_author_fax         '+ 34 981 167065'
_publ_contact_author_name        'De Blas, Andr\'es'
_publ_contact_author_phone       '+ 34 981 167000'
_publ_section_title
;
 Lanthanide(III) Complexes with Ligands Derived from a Cyclen Framework
 Containing Pyridinecarboxylate Pendants. The Effect of Steric Hindrance
 on the Hydration Number
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2509
_journal_page_last               2521
_journal_paper_doi               10.1021/ic202436j
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H28 N6 O4 Yb, F6 P, H2 O'
_chemical_formula_sum            'C22 H30 F6 N6 O5 P Yb'
_chemical_formula_weight         776.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-05-12T12:55:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.225(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5249(3)
_cell_length_b                   13.4108(5)
_cell_length_c                   20.5030(7)
_cell_measurement_reflns_used    9722
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3264
_cell_measurement_theta_min      2.5101
_cell_measurement_wavelength     0.71073
_cell_volume                     2603.54(16)
_computing_cell_refinement
'SAINT V7.68A (Bruker: Madison, 2009 ) in Apex2 suite'
_computing_data_collection       'Apex2, Bruker Instrument Service v2010, 1-2'
_computing_data_reduction
'SAINT and XPREP Version 2008/2 (Sheldrick, Bruker AXS Inc.)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'BRUKER-NONIUS X8 APEX KAPPA CCD'
_diffrn_measurement_method       'omega and  phi rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            57955
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         2
_exptl_absorpt_coefficient_mu    3.744
_exptl_absorpt_correction_T_max  0.492
_exptl_absorpt_correction_T_min  0.3673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        SADABS Version 2008/1 (Sheldrick, Bruker AXS Inc.)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.981
_exptl_crystal_description       prism
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.907
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.249
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+14.9776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.08
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                6094
_reflns_number_total             6479
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202436j_si_002.cif
_cod_data_source_block           1115341_b1_0s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'YES' changed to 'yes' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (7 times).

'_geom_angle_publ_flag' value 'YES'
changed to 'yes' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (28
times).

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4328417