Synthesis and X-ray Structure of the Mononuclear Nine-Coordinate Gadolinium(III) Hydrogen Oxydiacetate [Gd(C4H5O5)3].C4H6O5.H2O
Ricardo Baggio; Maria Teresa Garland; Mireille Perec; Inorganic Chemistry 36 (1997) 950–952; doi:10.1021/ic960974l

data_4323321
_publ_section_title
;
 Synthesis and X-ray Structure of the Mononuclear Nine-Coordinate
 Gadolinium(III) Hydrogen Oxydiacetate [Gd(C4H5O5)3].C4H6O5.H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              950
_journal_page_last               952
_journal_paper_doi               10.1021/ic960974l
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         '(Gd 3+), (C4 H5 O5 1-)3, (C4 H6 O5), (H2 O1)'
_chemical_formula_sum            'C16 H23 Gd O21'
_chemical_formula_weight         708.59
_chemical_name_common            ' Gadolinium(III) Hydrogen Oxydiacetate '
_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 (C-H) + difmap (O-H)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.90(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.566(3)
_cell_length_b                   25.171(13)
_cell_length_c                   14.710(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     2428(2)
_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_publication_material
;
CIFTAB (Sheldrick, 1993), PARST (Nardelli, 1983) and
CSD (Allen, Kennard & Taylor, 1983)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       '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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4668
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.830
_exptl_absorpt_correction_T_max  0.604
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   'Semiempirical ( Psi-scan)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1404
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_exptl_crystal_size_mid          0.32
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.120
_refine_ls_goodness_of_fit_obs   1.173
_refine_ls_hydrogen_treatment    'riding (C-H) + restrained refinement (O-H)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         4271
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.164
_refine_ls_restrained_S_obs      1.169
_refine_ls_R_factor_all          0.077
_refine_ls_R_factor_obs          0.047
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.8842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.132
_refine_ls_wR_factor_obs         0.112
_reflns_number_observed          3114
_reflns_number_total             4275
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960974l.cif
_cod_data_source_block           GdODA
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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 (41 time).

'_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 (23
times).

'_geom_angle_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 (36 times).

'_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
(94 times).

'_geom_torsion_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 (138 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.8842P] 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^)+(0.0636P)^2^+0.8842P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        2428.0(20)
_cod_database_code               4323321