Synthesis, Crystal Structure, and Magnetic Properties of the Mixed-Ligand Complex [Gd(CF3CO2)3(phen)2(H2O)]
Alberto Rizzi; Ricardo Baggio; Rafael Calvo; Maria T. Garland; Octavio Peña; Mireille Perec; Inorganic Chemistry 40 (2001) 3623–3625; doi:10.1021/ic001243v

data_4319931
_publ_section_title
;
 Synthesis, Crystal Structure, and Magnetic Properties of the Mixed-Ligand
 Complex [Gd(CF3CO2)3(phen)2(H2O)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3623
_journal_page_last               3625
_journal_paper_doi               10.1021/ic001243v
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety
' (Gd 2+), 3(C2 O2 F3 1-), 2(C12H8 N2), (H2 O) '
_chemical_formula_sum            'C30 H18 F9 Gd N4 O7'
_chemical_formula_weight         874.73
_chemical_name_systematic
; 
Aqua Tris(trifluoroacetate), bis(phenanthroline), gadolinium 
;
_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                76.689(13)
_cell_angle_beta                 85.589(14)
_cell_angle_gamma                62.898(12)
_cell_formula_units_Z            2
_cell_length_a                   11.889(2)
_cell_length_b                   12.158(2)
_cell_length_c                   13.225(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     1655.1(5)
_computing_cell_refinement       'Siemens P3/P4-PC version V4.27 (1991)'
_computing_data_collection       'Siemens P3/P4-PC version V4.27 (1991)'
_computing_data_reduction        'XDISK in SHELXTL/PC(Sheldrick,1991)'
_computing_molecular_graphics    'XP in SHELXTL/PC(Sheldrick,1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens R3m'
_diffrn_measurement_method       \w/2\q
_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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6179
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.106
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   \y-scan
_exptl_absorpt_process_details   'XEMP in SHELXTL/PC, Sheldrick,1991'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.891
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         5871
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          <0.01
_refine_ls_shift/su_mean         <0.01
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+1.8872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                5298
_reflns_number_total             5871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001243v.cif
_cod_data_source_block           TFA_GdPhen
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_angle_publ_flag' value 'N' changed to 'n' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (274 times).

'_geom_bond_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (19
times).

'_geom_bond_publ_flag' value 'N' changed to 'n' according to
the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (76 times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+1.8872P] 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^)+(0.0659P)^2^+1.8872P] 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        1655.2(5)
_cod_database_code               4319931