#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/14/2011448.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2011448
loop_
_publ_author_name
'Farrugia, Louis J.'
'Peacock, Robert D.'
'Stewart, Brian'
_publ_section_title
;
 Lanthanide complexes of 2,2'-oxydiacetate:
 Na₅[M(C₄H₄O₅)₃](BF₄)₂·6H₂O (M =
 Nd, Sm or Gd)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e435
_journal_page_last               e436
_journal_paper_doi               10.1107/S0108270100012087
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          'Na5 [Gd (C4 H4 O5)3] (B F4)2, 6H2 O'
_chemical_formula_moiety
'5Na 1+, C12 H12 Gd O15 3-, 2B1 F4 1-, 6H2 O1'
_chemical_formula_structural     'C12 H24 B2 F8 Gd Na5 O21'
_chemical_formula_sum            'C12 H24 B2 F8 Gd Na5 O21'
_chemical_formula_weight         950.13
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   9.7041(10)
_cell_length_b                   9.7041(10)
_cell_length_c                   28.025(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      15.2
_cell_measurement_theta_min      12.1
_cell_volume                     2285.5(6)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Enraf Nonius CAD-4'
_diffrn_measurement_method       'non-profiled ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .013
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            2033
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.381
_exptl_absorpt_correction_T_max  .433
_exptl_absorpt_correction_T_min  .336
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1395
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .45
_exptl_crystal_size_min          .35
_refine_diff_density_max         .38
_refine_diff_density_min         -.26
_refine_ls_abs_structure_details 'Flack (1983), 206 Friedel pairs'
_refine_ls_abs_structure_Flack   -.005(10)
_refine_ls_extinction_coef       .00258(15)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          .012
_refine_ls_R_factor_gt           .012
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0226P)²+0.5279P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .032
_reflns_number_gt                1078
_reflns_number_total             1078
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qa0369.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               2011448
_cod_database_fobs_code          2011448
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Gd1 0 0 0 .01797(6) Uani d S 1 . . Gd
O1 -.2566(2) -.2566(2) 0 .0279(4) Uani d S 1 . . O
O2 -.19123(16) -.02868(17) -.05864(5) .0283(3) Uani d . 1 . . O
O3 -.4154(2) -.1616(2) -.09977(5) .0404(4) Uani d . 1 . . O
C1 -.3823(2) -.2874(3) -.03196(7) .0319(4) Uani d . 1 . . C
H1A -.4746 -.3022 -.0142 .038 Uiso calc R 1 . . H
H1B -.4122 -.384 -.0498 .038 Uiso calc R 1 . . H
C2 -.32749(19) -.1480(4) -.06592(5) .0251(6) Uani d . 1 . . C
B1 -.3333 .3333 -.23679(12) .0393(7) Uani d S 1 . . B
F1 -.3333 .3333 -.28550(8) .0783(9) Uani d S 1 . . F
F2 -.2482(5) .2641(5) -.21977(7) .0668(5) Uani d . 1 . . F
Na1 -.6667 -.3333 -.13370(4) .0309(2) Uani d S 1 . . Na
Na2 -.3333 .04815(18) -.1667 .0499(4) Uani d S 1 . . Na
O4 -.5922(2) -.1134(2) -.19064(6) .0418(4) Uani d . 1 . . O
H41 -.5676 -.1335 -.2193 .079(8) Uiso d R 1 . . H
H42 -.5854 -.0383 -.2018 .079(8) Uiso d R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Gd Gd -.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na .0362 .0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-4 1 -11
3 0 -12
2 -5 -5
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2 Gd1 O2 6 . 148.44(7)
O2 Gd1 O2 6 2 126.94(7)
O2 Gd1 O2 . 2 77.87(5)
O2 Gd1 O2 6 5 77.87(5)
O2 Gd1 O2 . 5 88.12(7)
O2 Gd1 O2 2 5 148.44(7)
O2 Gd1 O2 6 3 88.12(7)
O2 Gd1 O2 . 3 77.87(5)
O2 Gd1 O2 2 3 77.87(5)
O2 Gd1 O2 5 3 126.94(7)
O2 Gd1 O2 6 4 77.87(5)
O2 Gd1 O2 . 4 126.94(7)
O2 Gd1 O2 2 4 88.12(7)
O2 Gd1 O2 5 4 77.87(5)
O2 Gd1 O2 3 4 148.44(7)
O2 Gd1 O1 6 . 135.94(3)
O2 Gd1 O1 . . 63.47(3)
O2 Gd1 O1 2 . 74.22(4)
O2 Gd1 O1 5 . 74.22(4)
O2 Gd1 O1 3 . 135.94(3)
O2 Gd1 O1 4 . 63.47(3)
O2 Gd1 O1 6 2 63.47(3)
O2 Gd1 O1 . 2 135.94(3)
O2 Gd1 O1 2 2 63.47(3)
O2 Gd1 O1 5 2 135.94(3)
O2 Gd1 O1 3 2 74.22(4)
O2 Gd1 O1 4 2 74.22(4)
O1 Gd1 O1 . 2 120
O2 Gd1 O1 6 3 74.22(4)
O2 Gd1 O1 . 3 74.22(4)
O2 Gd1 O1 2 3 135.94(3)
O2 Gd1 O1 5 3 63.47(3)
O2 Gd1 O1 3 3 63.47(3)
O2 Gd1 O1 4 3 135.94(3)
O1 Gd1 O1 . 3 120
O1 Gd1 O1 2 3 120
C1 O1 C1 . 4 115.3(2)
C1 O1 Gd1 . . 122.36(11)
C1 O1 Gd1 4 . 122.36(11)
C2 O2 Gd1 . . 127.83(15)
C2 O3 Na1 . . 142.97(18)
C2 O3 Na2 . . 123.19(17)
Na1 O3 Na2 . . 93.82(5)
O1 C1 C2 . . 109.07(15)
O3 C2 O2 . . 124.8(3)
O3 C2 C1 . . 118.0(2)
O2 C2 C1 . . 117.09(17)
F1 B1 F2 . . 110.16(15)
F1 B1 F2 . 2_565 110.16(15)
F2 B1 F2 . 2_565 108.78(16)
F1 B1 F2 . 3_455 110.16(15)
F2 B1 F2 . 3_455 108.78(16)
F2 B1 F2 2_565 3_455 108.78(16)
B1 F2 Na2 . . 128.3(3)
O3 Na1 O3 2_455 . 104.84(5)
O3 Na1 O3 2_455 3_445 104.84(5)
O3 Na1 O3 . 3_445 104.84(5)
O3 Na1 O4 2_455 . 85.80(6)
O3 Na1 O4 . . 84.12(6)
O3 Na1 O4 3_445 . 163.41(7)
O3 Na1 O4 2_455 2_455 84.12(6)
O3 Na1 O4 . 2_455 163.41(7)
O3 Na1 O4 3_445 2_455 85.80(6)
O4 Na1 O4 . 2_455 82.64(6)
O3 Na1 O4 2_455 3_445 163.41(7)
O3 Na1 O4 . 3_445 85.80(6)
O3 Na1 O4 3_445 3_445 84.12(6)
O4 Na1 O4 . 3_445 82.64(6)
O4 Na1 O4 2_455 3_445 82.64(6)
O3 Na1 Na2 2_455 2_455 45.52(4)
O3 Na1 Na2 . 2_455 145.60(5)
O3 Na1 Na2 3_445 2_455 100.65(5)
O4 Na1 Na2 . 2_455 77.53(5)
O4 Na1 Na2 2_455 2_455 39.00(4)
O4 Na1 Na2 3_445 2_455 119.76(5)
O3 Na1 Na2 2_455 . 100.65(5)
O3 Na1 Na2 . . 45.52(4)
O3 Na1 Na2 3_445 . 145.60(5)
O4 Na1 Na2 . . 39.00(4)
O4 Na1 Na2 2_455 . 119.76(5)
O4 Na1 Na2 3_445 . 77.53(5)
Na2 Na1 Na2 2_455 . 113.693(15)
O3 Na1 Na2 2_455 3_445 145.60(5)
O3 Na1 Na2 . 3_445 100.65(5)
O3 Na1 Na2 3_445 3_445 45.52(4)
O4 Na1 Na2 . 3_445 119.76(5)
O4 Na1 Na2 2_455 3_445 77.53(5)
O4 Na1 Na2 3_445 3_445 39.00(4)
Na2 Na1 Na2 2_455 3_445 113.693(15)
Na2 Na1 Na2 . 3_445 113.693(15)
O4 Na2 O4 . 18_444 164.42(13)
O4 Na2 F2 . 18_444 89.66(11)
O4 Na2 F2 18_444 18_444 101.50(12)
O4 Na2 F2 . . 101.50(12)
O4 Na2 F2 18_444 . 89.66(11)
F2 Na2 F2 18_444 . 88.91(11)
O4 Na2 O3 . . 82.73(7)
O4 Na2 O3 18_444 . 87.41(6)
F2 Na2 O3 18_444 . 85.03(6)
F2 Na2 O3 . . 172.60(10)
O4 Na2 O3 . 18_444 87.41(6)
O4 Na2 O3 18_444 18_444 82.73(7)
F2 Na2 O3 18_444 18_444 172.60(10)
F2 Na2 O3 . 18_444 85.03(6)
O3 Na2 O3 . 18_444 101.32(10)
O4 Na2 Na1 . . 42.47(5)
O4 Na2 Na1 18_444 . 125.54(7)
F2 Na2 Na1 18_444 . 90.87(7)
F2 Na2 Na1 . . 143.97(10)
O3 Na2 Na1 . . 40.66(4)
O3 Na2 Na1 18_444 . 91.55(6)
O4 Na2 Na1 . 16_554 125.54(7)
O4 Na2 Na1 18_444 16_554 42.47(5)
F2 Na2 Na1 18_444 16_554 143.97(10)
F2 Na2 Na1 . 16_554 90.87(7)
O3 Na2 Na1 . 16_554 91.55(6)
O3 Na2 Na1 18_444 16_554 40.65(4)
Na1 Na2 Na1 . 16_554 109.50(5)
Na2 O4 Na1 . . 98.53(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Gd1 O2 6 2.3887(13) ?
Gd1 O2 . 2.3887(13) ?
Gd1 O2 2 2.3887(13) ?
Gd1 O2 5 2.3887(13) ?
Gd1 O2 3 2.3887(13) ?
Gd1 O2 4 2.3887(13) ?
Gd1 O1 . 2.490(2) ?
Gd1 O1 2 2.490(2) ?
Gd1 O1 3 2.490(2) ?
O1 C1 . 1.420(2) ?
O1 C1 4 1.420(2) ?
O2 C2 . 1.265(2) ?
O3 C2 . 1.238(2) ?
O3 Na1 . 2.3585(16) ?
O3 Na2 . 2.583(2) ?
C1 C2 . 1.516(4) ?
B1 F1 . 1.365(4) ?
B1 F2 . 1.384(2) ?
B1 F2 2_565 1.384(2) ?
B1 F2 3_455 1.384(2) ?
F2 Na2 . 2.358(4) ?
Na1 O3 2_455 2.3585(16) ?
Na1 O3 3_445 2.3585(16) ?
Na1 O4 . 2.466(2) ?
Na1 O4 2_455 2.466(2) ?
Na1 O4 3_445 2.466(2) ?
Na1 Na2 2_455 3.6120(11) ?
Na1 Na2 . 3.6120(11) ?
Na1 Na2 3_445 3.6120(11) ?
Na2 O4 . 2.2985(18) ?
Na2 O4 18_444 2.2985(18) ?
Na2 F2 18_444 2.357(4) ?
Na2 O3 18_444 2.583(2) ?
Na2 Na1 16_554 3.6121(11) ?
