#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:38:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179416 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/13/4331318.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4331318
loop_
_publ_author_name
'Xiao-Yan Chen'
'George S. Goff'
'William C. Ewing'
'Brian L. Scott'
'Wolfgang Runde'
_publ_section_title
;
 Solid-State and Solution-State Coordination Chemistry of Lanthanide(III)
 Complexes with α-Hydroxyisobutyric Acid
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13254
_journal_page_last               13263
_journal_paper_doi               10.1021/ic301775d
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C8 H20 Gd N O12'
_chemical_formula_weight         479.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 92.5150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8635(10)
_cell_length_b                   8.4868(9)
_cell_length_c                   20.917(2)
_cell_measurement_temperature    120(1)
_cell_volume                     1571.9(3)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8501
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.279
_exptl_absorpt_correction_T_max  0.9193
_exptl_absorpt_correction_T_min  0.5857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_description       'rectanglar plate'
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0201
_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/[σ²(Fo²)+(0.0289P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0513
_reflns_number_gt                1739
_reflns_number_total             1846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301775d_si_001_7.cif
_cod_data_source_block           apx1466
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4331318
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Gd1 Gd 0.0000 0.39933(2) 0.2500 0.00850(7) Uani 1 2 d S
N1 N 0.6743(5) 0.1798(6) 0.0216(2) 0.0128(9) Uani 0.50 1 d P
O1 O -0.0095(2) 0.2612(3) 0.14887(10) 0.0168(5) Uani 1 1 d .
O2 O 0.1849(2) 0.2040(2) 0.23644(9) 0.0156(4) Uani 1 1 d .
O3 O 0.2872(2) -0.0021(2) 0.18843(9) 0.0135(4) Uani 1 1 d .
O4 O 0.1068(3) 0.5856(2) 0.18152(10) 0.0197(5) Uani 1 1 d .
O5 O 0.5797(3) 0.0888(3) 0.05089(12) 0.0325(6) Uani 1 1 d .
O6 O 0.6830(6) 0.1814(7) -0.0382(2) 0.0205(11) Uani 0.50 1 d P
O6' O 0.7615(6) 0.2683(6) 0.0541(3) 0.0207(11) Uani 0.50 1 d P
C1 C 0.0855(3) 0.1301(3) 0.13245(14) 0.0120(6) Uani 1 1 d .
C2 C -0.0105(4) -0.0162(4) 0.12220(16) 0.0206(6) Uani 1 1 d .
H2A H -0.0665 -0.0357 0.1596 0.031 Uiso 1 1 calc R
H2B H 0.0535 -0.1048 0.1145 0.031 Uiso 1 1 calc R
H2C H -0.0793 -0.0008 0.0860 0.031 Uiso 1 1 calc R
C3 C 0.1726(3) 0.1711(4) 0.07364(14) 0.0194(6) Uani 1 1 d .
H3A H 0.1040 0.1771 0.0369 0.029 Uiso 1 1 calc R
H3B H 0.2467 0.0911 0.0668 0.029 Uiso 1 1 calc R
H3C H 0.2220 0.2708 0.0800 0.029 Uiso 1 1 calc R
C4 C 0.1945(3) 0.1081(3) 0.19035(14) 0.0125(6) Uani 1 1 d .
H1 H -0.057(6) 0.268(7) 0.124(3) 0.080 Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Gd1 O2 90.63(10) 2 .
O2 Gd1 O4 95.66(8) 2 2
O2 Gd1 O4 147.56(7) . 2
O2 Gd1 O4 147.56(7) 2 .
O2 Gd1 O4 95.66(8) . .
O4 Gd1 O4 95.84(11) 2 .
O2 Gd1 O3 135.93(6) 2 4
O2 Gd1 O3 76.95(7) . 4
O4 Gd1 O3 76.48(7) 2 4
O4 Gd1 O3 76.37(7) . 4
O2 Gd1 O3 76.95(7) 2 3_455
O2 Gd1 O3 135.92(6) . 3_455
O4 Gd1 O3 76.37(7) 2 3_455
O4 Gd1 O3 76.47(7) . 3_455
O3 Gd1 O3 138.99(9) 4 3_455
O2 Gd1 O1 63.34(7) 2 2
O2 Gd1 O1 76.49(7) . 2
O4 Gd1 O1 78.07(8) 2 2
O4 Gd1 O1 148.98(7) . 2
O3 Gd1 O1 72.63(7) 4 2
O3 Gd1 O1 129.67(7) 3_455 2
O2 Gd1 O1 76.49(7) 2 .
O2 Gd1 O1 63.34(7) . .
O4 Gd1 O1 148.98(7) 2 .
O4 Gd1 O1 78.07(8) . .
O3 Gd1 O1 129.67(7) 4 .
O3 Gd1 O1 72.63(7) 3_455 .
O1 Gd1 O1 121.96(11) 2 .
O6' N1 O6 118.0(5) . .
O6' N1 O5 119.3(5) . .
O6 N1 O5 122.6(5) . .
O6' N1 O6 21.4(3) . 7_655
O6 N1 O6 96.6(4) . 7_655
O5 N1 O6 140.7(4) . 7_655
O6' N1 O6' 97.0(4) . 7_655
O6 N1 O6' 21.0(3) . 7_655
O5 N1 O6' 143.6(4) . 7_655
O6 N1 O6' 75.6(3) 7_655 7_655
C1 O1 Gd1 125.66(16) . .
C1 O1 H1 104(5) . .
Gd1 O1 H1 130(5) . .
C4 O2 Gd1 127.84(18) . .
C4 O3 Gd1 138.71(19) . 3_545
O6' O6 N1 121.6(8) 7_655 .
O6' O6 N1 38.2(6) 7_655 7_655
N1 O6 N1 83.4(4) . 7_655
O6 O6' N1 120.4(8) 7_655 .
O6 O6' N1 37.4(6) 7_655 7_655
N1 O6' N1 83.0(4) . 7_655
O1 C1 C2 109.6(2) . .
O1 C1 C3 109.8(2) . .
C2 C1 C3 112.0(2) . .
O1 C1 C4 105.1(2) . .
C2 C1 C4 110.1(2) . .
C3 C1 C4 110.1(2) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
O3 C4 O2 124.9(3) . .
O3 C4 C1 117.5(2) . .
O2 C4 C1 117.6(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 O2 2.3571(19) 2
Gd1 O2 2.3571(19) .
Gd1 O4 2.359(2) 2
Gd1 O4 2.359(2) .
Gd1 O3 2.3879(19) 4
Gd1 O3 2.3880(19) 3_455
Gd1 O1 2.417(2) 2
Gd1 O1 2.417(2) .
N1 O6' 1.256(7) .
N1 O6 1.257(7) .
N1 O5 1.312(6) .
N1 O6 1.752(7) 7_655
N1 O6' 1.762(7) 7_655
O1 C1 1.445(3) .
O1 H1 0.66(5) .
O2 C4 1.267(3) .
O3 C4 1.247(3) .
O3 Gd1 2.3879(19) 3_545
O6 O6' 0.741(5) 7_655
O6 N1 1.752(7) 7_655
O6' O6 0.741(5) 7_655
O6' N1 1.762(7) 7_655
C1 C2 1.515(4) .
C1 C3 1.521(4) .
C1 C4 1.528(4) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
