 
data_1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C H Gd O4' 
_chemical_formula_weight          234.27 
 
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' 
 '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' 
 
_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    Pnma
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 'x+1/2, -y+1/2, -z+1/2' 
 '-x, y+1/2, -z' 
 '-x, -y, -z' 
 'x-1/2, y, -z-1/2' 
 '-x-1/2, y-1/2, z-1/2' 
 'x, -y-1/2, z' 
 
_cell_length_a                    7.0770(7) 
_cell_length_b                    4.8730(9) 
_cell_length_c                    8.4353(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      290.90(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     418 
_cell_measurement_theta_min       9.67
_cell_measurement_theta_max       52.44 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     5.349 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              412 
_exptl_absorpt_coefficient_mu     22.608 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.0931 
_exptl_absorpt_correction_T_max   0.0931 
_exptl_absorpt_process_details    '(ABSCOR; Higashi, 1995)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             2591 
_diffrn_reflns_av_R_equivalents   0.0305 
_diffrn_reflns_av_sigmaI/netI     0.0153 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -6 
_diffrn_reflns_limit_k_max        6 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        10 
_diffrn_reflns_theta_min          3.76 
_diffrn_reflns_theta_max          26.99 
_reflns_number_total              356 
_reflns_number_gt                 346 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection      'PROCESS-AUTO (Rigaku, 1998)'
_computing_cell_refinement      'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction       'PROCESS-AUTO (Rigaku, 1998)'
_computing_structure_solution   'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0184P)²+10.1786P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.038(2) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          356 
_refine_ls_number_parameters      35 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0208 
_refine_ls_R_factor_gt            0.0201 
_refine_ls_wR_factor_ref          0.0538 
_refine_ls_wR_factor_gt           0.0533 
_refine_ls_goodness_of_fit_ref    1.036 
_refine_ls_restrained_S_all       1.036 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
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 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Gd1 Gd 0.36013(6) -0.2500 0.33507(6) 0.0070(3) Uani 1 2 d S . . 
O1 O 0.5407(11) -0.2500 0.1101(9) 0.0130(16) Uani 1 2 d S . . 
H1A H 0.4899 -0.2500 0.0058 0.016 Uiso 1 2 d SR . . 
O2 O 0.1538(7) 0.0233(11) 0.1080(6) 0.0108(10) Uani 1 1 d . . . 
O3 O 0.2972(11) 0.2500 0.2990(9) 0.0137(16) Uani 1 2 d S . . 
C1 C 0.1985(14) 0.2500 0.1736(12) 0.0074(18) Uani 1 2 d S . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Gd1 0.0062(3) 0.0059(3) 0.0089(3) 0.000 0.00082(17) 0.000 
O1 0.010(3) 0.019(4) 0.010(4) 0.000 -0.001(3) 0.000 
O2 0.012(2) 0.007(2) 0.014(2) -0.004(2) 0.0026(18) -0.003(2) 
O3 0.016(4) 0.011(4) 0.014(4) 0.000 -0.006(3) 0.000 
C1 0.007(4) 0.007(4) 0.008(4) 0.000 0.001(4) 0.000 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Gd1 O1 2.288(8) . ? 
Gd1 O1 2.307(7) 6_556 ? 
Gd1 O3 2.4955(17) 1_545 ? 
Gd1 O3 2.4955(17) . ? 
Gd1 O2 2.515(5) 6_656 ? 
Gd1 O2 2.515(5) 3_545 ? 
Gd1 O2 2.555(5) 2 ? 
Gd1 O2 2.555(5) 7_656 ? 
Gd1 O2 2.752(5) 8 ? 
Gd1 O2 2.752(5) . ? 
Gd1 C1 2.886(10) 2 ? 
Gd1 C1 3.016(6) 1_545 ? 
O1 Gd1 2.307(7) 6_656 ? 
O1 H1A 0.9500 . ? 
O2 C1 1.276(7) . ? 
O2 Gd1 2.515(5) 6_556 ? 
O2 Gd1 2.555(5) 2_554 ? 
O3 C1 1.267(13) . ? 
O3 Gd1 2.4955(17) 1_565 ? 
C1 O2 1.276(7) 8_565 ? 
C1 Gd1 2.886(10) 2_554 ? 
C1 Gd1 3.016(6) 1_565 ? 
 
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 
 _geom_angle_publ_flag 
O1 Gd1 O1 135.5(2) . 6_556 ? 
O1 Gd1 O3 89.91(19) . 1_545 ? 
O1 Gd1 O3 81.35(19) 6_556 1_545 ? 
O1 Gd1 O3 89.91(19) . . ? 
O1 Gd1 O3 81.35(19) 6_556 . ? 
O3 Gd1 O3 155.0(3) 1_545 . ? 
O1 Gd1 O2 72.4(2) . 6_656 ? 
O1 Gd1 O2 140.47(16) 6_556 6_656 ? 
O3 Gd1 O2 133.5(2) 1_545 6_656 ? 
O3 Gd1 O2 69.7(2) . 6_656 ? 
O1 Gd1 O2 72.4(2) . 3_545 ? 
O1 Gd1 O2 140.47(16) 6_556 3_545 ? 
O3 Gd1 O2 69.7(2) 1_545 3_545 ? 
O3 Gd1 O2 133.5(2) . 3_545 ? 
O2 Gd1 O2 64.0(2) 6_656 3_545 ? 
O1 Gd1 O2 140.24(18) . 2 ? 
O1 Gd1 O2 77.4(2) 6_556 2 ? 
O3 Gd1 O2 121.7(2) 1_545 2 ? 
O3 Gd1 O2 71.4(2) . 2 ? 
O2 Gd1 O2 68.33(19) 6_656 2 ? 
O2 Gd1 O2 95.09(12) 3_545 2 ? 
O1 Gd1 O2 140.24(18) . 7_656 ? 
O1 Gd1 O2 77.4(2) 6_556 7_656 ? 
O3 Gd1 O2 71.4(2) 1_545 7_656 ? 
O3 Gd1 O2 121.7(2) . 7_656 ? 
O2 Gd1 O2 95.09(12) 6_656 7_656 ? 
O2 Gd1 O2 68.33(19) 3_545 7_656 ? 
O2 Gd1 O2 51.2(2) 2 7_656 ? 
O1 Gd1 O2 73.69(19) . 8 ? 
O1 Gd1 O2 67.66(19) 6_556 8 ? 
O3 Gd1 O2 49.3(2) 1_545 8 ? 
O3 Gd1 O2 107.0(2) . 8 ? 
O2 Gd1 O2 145.87(12) 6_656 8 ? 
O2 Gd1 O2 108.37(18) 3_545 8 ? 
O2 Gd1 O2 144.66(8) 2 8 ? 
O2 Gd1 O2 113.41(5) 7_656 8 ? 
O1 Gd1 O2 73.69(19) . . ? 
O1 Gd1 O2 67.66(19) 6_556 . ? 
O3 Gd1 O2 107.0(2) 1_545 . ? 
O3 Gd1 O2 49.3(2) . . ? 
O2 Gd1 O2 108.37(18) 6_656 . ? 
O2 Gd1 O2 145.87(12) 3_545 . ? 
O2 Gd1 O2 113.41(5) 2 . ? 
O2 Gd1 O2 144.66(8) 7_656 . ? 
O2 Gd1 O2 57.9(2) 8 . ? 
O1 Gd1 C1 154.3(3) . 2 ? 
O1 Gd1 C1 70.2(3) 6_556 2 ? 
O3 Gd1 C1 95.45(18) 1_545 2 ? 
O3 Gd1 C1 95.45(18) . 2 ? 
O2 Gd1 C1 86.0(2) 6_656 2 ? 
O2 Gd1 C1 86.0(2) 3_545 2 ? 
O2 Gd1 C1 26.23(12) 2 2 ? 
O2 Gd1 C1 26.23(12) 7_656 2 ? 
O2 Gd1 C1 127.76(19) 8 2 ? 
O2 Gd1 C1 127.76(19) . 2 ? 
O1 Gd1 C1 80.6(2) . 1_545 ? 
O1 Gd1 C1 73.7(2) 6_556 1_545 ? 
O3 Gd1 C1 24.3(2) 1_545 1_545 ? 
O3 Gd1 C1 131.8(2) . 1_545 ? 
O2 Gd1 C1 145.8(2) 6_656 1_545 ? 
O2 Gd1 C1 88.4(2) 3_545 1_545 ? 
O2 Gd1 C1 137.8(2) 2 1_545 ? 
O2 Gd1 C1 92.5(2) 7_656 1_545 ? 
O2 Gd1 C1 25.02(19) 8 1_545 ? 
O2 Gd1 C1 82.85(19) . 1_545 ? 
C1 Gd1 C1 113.09(16) 2 1_545 ? 
Gd1 O1 Gd1 112.4(3) . 6_656 ? 
Gd1 O1 H1A 123.8 . . ? 
Gd1 O1 H1A 123.8 6_656 . ? 
C1 O2 Gd1 125.5(5) . 6_556 ? 
C1 O2 Gd1 91.5(5) . 2_554 ? 
Gd1 O2 Gd1 111.67(19) 6_556 2_554 ? 
C1 O2 Gd1 89.1(5) . . ? 
Gd1 O2 Gd1 92.82(17) 6_556 . ? 
Gd1 O2 Gd1 148.9(2) 2_554 . ? 
C1 O3 Gd1 101.54(18) . 1_565 ? 
C1 O3 Gd1 101.54(18) . . ? 
Gd1 O3 Gd1 155.0(3) 1_565 . ? 
O3 C1 O2 119.9(4) . . ? 
O3 C1 O2 119.9(4) . 8_565 ? 
O2 C1 O2 120.0(9) . 8_565 ? 
O3 C1 Gd1 154.8(7) . 2_554 ? 
O2 C1 Gd1 62.3(5) . 2_554 ? 
O2 C1 Gd1 62.3(5) 8_565 2_554 ? 
O3 C1 Gd1 54.15(16) . 1_565 ? 
O2 C1 Gd1 171.7(6) . 1_565 ? 
O2 C1 Gd1 65.8(3) 8_565 1_565 ? 
Gd1 C1 Gd1 120.08(19) 2_554 1_565 ? 
O3 C1 Gd1 54.15(16) . . ? 
O2 C1 Gd1 65.8(3) . . ? 
O2 C1 Gd1 171.7(6) 8_565 . ? 
Gd1 C1 Gd1 120.08(19) 2_554 . ? 
Gd1 C1 Gd1 107.8(3) 1_565 . ? 
 
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              26.99 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    1.215 
_refine_diff_density_min   -0.945 
_refine_diff_density_rms    0.271 
