#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/23/2212351.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_2212351
loop_
_publ_author_name
'Shao-Ming Ying'
'Jian-Qiang Liu'
'Shuang-Lian Cai'
'Fan Zhong'
'Guang-Pei Zhou'
_publ_section_title
;Poly[[diaqua[μ₆-(butane-1,4-diyldinitrilotetramethylene)tetraphosphonato]di-μ₂-oxalato-digadolinium(III)]
 tetrahydrate]
;
_journal_coeditor_code           SA2032
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m415
_journal_page_last               m417
_journal_paper_doi               10.1107/S1600536807000049
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Gd2 (C2 O4)2 (C8 H22 O12 N2 P4) (H2 O)2] , 4H2 O'
_chemical_formula_sum            'C6 H17 Gd N O13 P2'
_chemical_formula_weight         530.40
_chemical_name_systematic
;
catena Poly[diaqua bis(oxalic acid) (tetramethylphosphono-1,4-diaminobutane)
digadolinium(III)] tetrahydrate
;
_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           SHELXL97
_cell_angle_alpha                106.939(3)
_cell_angle_beta                 98.292(3)
_cell_angle_gamma                110.123(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5191(6)
_cell_length_b                   9.6282(6)
_cell_length_c                   9.6452(6)
_cell_measurement_reflns_used    2718
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.699
_cell_measurement_theta_min      2.294
_cell_volume                     764.05(9)
_computing_cell_refinement       'SMART (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0790
_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       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6629
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         2.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.618
_exptl_absorpt_correction_T_max  0.8933
_exptl_absorpt_correction_T_min  0.3867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.780
_refine_diff_density_min         -1.919
_refine_ls_extinction_coef       0.0049(8)
_refine_ls_extinction_method     'SHELXL (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2728
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0446
_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)+(0.0597P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                2140
_reflns_number_total             2728
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sa2032.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        764.05(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2212351
_cod_database_fobs_code          2212351
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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
Gd Gd1 0.58737(5) 0.72593(4) 0.81782(4) 0.02119(15) Uani d . 1
P P1 0.2630(3) 0.4901(2) 0.4847(2) 0.0234(5) Uani d . 1
P P2 0.2393(3) 0.9714(2) 0.3473(3) 0.0297(5) Uani d . 1
N N1 0.2567(9) 0.6690(8) 0.3055(8) 0.0276(18) Uani d . 1
H H1A 0.312(9) 0.625(9) 0.276(8) 0.02(2) Uiso d . 1
O O7 0.4647(7) 0.6667(6) 1.0071(6) 0.0338(14) Uani d . 1
O O8 0.6016(7) 1.1558(6) 1.1714(6) 0.0307(13) Uani d . 1
O O9 0.4134(7) 0.5155(6) 1.1446(6) 0.0308(14) Uani d . 1
O O10 0.6749(6) 0.9783(6) 1.0313(6) 0.0303(14) Uani d . 1
O O1 0.0893(6) 0.3920(6) 0.4747(7) 0.0363(15) Uani d . 1
H H1 0.0525 0.3106 0.3991 0.054 Uiso calc R 1
O O2 0.3090(6) 0.4033(6) 0.3569(6) 0.0258(13) Uani d . 1
O O3 0.3573(6) 0.5350(6) 0.6421(6) 0.0261(13) Uani d . 1
O O6 0.0686(7) 0.9018(7) 0.2696(8) 0.0473(17) Uani d . 1
O O5 0.3374(7) 1.1078(6) 0.3124(7) 0.0377(15) Uani d . 1
O O4 0.2726(8) 1.0112(7) 0.5199(7) 0.0459(18) Uani d . 1
H H4 0.2506 1.0860 0.5588 0.069 Uiso calc R 1
O O13 0.8584(8) 0.7984(8) 0.9529(8) 0.0448(16) Uani d D 1
H H13B 0.9171 0.8336 0.9053 0.067 Uiso calc RD 1
H H13A 0.888(14) 0.822(14) 1.047(4) 0.10(5) Uiso d D 1
O O12 0.7750(9) 0.7605(8) 0.2989(7) 0.0503(18) Uani d D 1
H H12B 0.7705 0.6848 0.3306 0.07(4) Uiso d RD 1
H H12A 0.8709 0.8111 0.3077 0.08(4) Uiso d RD 1
O O11 0.0404(7) 0.8710(7) 0.7654(7) 0.0463(17) Uani d D 1
H H11B 0.1328 0.9118 0.8241 0.08(4) Uiso d RD 1
H H11A 0.0217 0.9423 0.7425 0.09(5) Uiso d RD 1
C C1 0.0787(11) 0.5600(10) 0.0478(10) 0.045(3) Uani d . 1
H H12 0.0944 0.6628 0.0417 0.054 Uiso calc R 1
H H11 0.1576 0.5291 0.0118 0.054 Uiso calc R 1
C C2 0.0938(10) 0.5714(9) 0.2129(9) 0.035(2) Uani d . 1
H H22 0.0266 0.6188 0.2537 0.042 Uiso calc R 1
H H21 0.0607 0.4656 0.2164 0.042 Uiso calc R 1
C C3 0.3293(10) 0.8288(9) 0.2943(10) 0.030(2) Uani d . 1
H H32 0.3332 0.8114 0.1909 0.036 Uiso calc R 1
H H31 0.4359 0.8796 0.3564 0.036 Uiso calc R 1
C C4 0.2774(11) 0.6785(9) 0.4664(9) 0.032(2) Uani d . 1
H H42 0.1985 0.7073 0.5048 0.038 Uiso calc R 1
H H41 0.3783 0.7614 0.5273 0.038 Uiso calc R 1
C C5 0.5786(9) 1.0380(8) 1.0576(9) 0.0257(19) Uani d . 1
C C6 0.4646(9) 0.5530(9) 1.0430(9) 0.0215(18) Uani d . 1
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'
P P 0.1023 0.0942 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O5 Gd1 O3 2_676 . 98.9(2)
O5 Gd1 O2 2_676 2_666 76.27(18)
O3 Gd1 O2 . 2_666 80.85(19)
O5 Gd1 O7 2_676 . 148.5(2)
O3 Gd1 O7 . . 86.62(19)
O2 Gd1 O7 2_666 . 135.15(17)
O5 Gd1 O8 2_676 2_677 78.21(19)
O3 Gd1 O8 . 2_677 73.57(18)
O2 Gd1 O8 2_666 2_677 140.25(18)
O7 Gd1 O8 . 2_677 73.66(18)
O5 Gd1 O9 2_676 2_667 145.7(2)
O3 Gd1 O9 . 2_667 79.08(18)
O2 Gd1 O9 2_666 2_667 69.60(17)
O7 Gd1 O9 . 2_667 65.78(18)
O8 Gd1 O9 2_677 2_667 131.85(19)
O5 Gd1 O10 2_676 . 82.8(2)
O3 Gd1 O10 . . 138.43(18)
O2 Gd1 O10 2_666 . 138.35(19)
O7 Gd1 O10 . . 73.11(19)
O8 Gd1 O10 2_677 . 66.11(18)
O9 Gd1 O10 2_667 . 121.41(18)
O5 Gd1 O13 2_676 . 92.9(2)
O3 Gd1 O13 . . 148.7(2)
O2 Gd1 O13 2_666 . 73.9(2)
O7 Gd1 O13 . . 98.3(2)
O8 Gd1 O13 2_677 . 137.6(2)
O9 Gd1 O13 2_667 . 75.0(2)
O10 Gd1 O13 . . 71.68(19)
O2 P1 O3 . . 118.3(3)
O2 P1 O1 . . 110.0(3)
O3 P1 O1 . . 107.2(3)
O2 P1 C4 . . 107.7(3)
O3 P1 C4 . . 105.3(3)
O1 P1 C4 . . 107.9(4)
O5 P2 O6 . . 115.2(4)
O5 P2 O4 . . 111.2(3)
O6 P2 O4 . . 112.6(4)
O5 P2 C3 . . 102.7(3)
O6 P2 C3 . . 113.1(4)
O4 P2 C3 . . 100.6(4)
C2 N1 C3 . . 115.1(6)
C2 N1 C4 . . 112.2(7)
C3 N1 C4 . . 112.4(6)
C2 N1 H1A . . 110(5)
C3 N1 H1A . . 103(5)
C4 N1 H1A . . 103(5)
C6 O7 Gd1 . . 120.5(5)
C5 O8 Gd1 . 2_677 119.6(5)
C6 O9 Gd1 . 2_667 120.2(5)
C5 O10 Gd1 . . 118.5(5)
P1 O1 H1 . . 109.5
P1 O2 Gd1 . 2_666 171.8(3)
P1 O3 Gd1 . . 141.1(3)
P2 O5 Gd1 . 2_676 159.0(4)
P2 O4 H4 . . 109.5
Gd1 O13 H13B . . 109.5
Gd1 O13 H13A . . 123(9)
H13B O13 H13A . . 122.3
H12B O12 H12A . . 105.7
H11B O11 H11A . . 109.4
C1 C1 C2 2_565 . 109.4(10)
C1 C1 H12 2_565 . 109.8
C2 C1 H12 . . 109.8
C1 C1 H11 2_565 . 109.8
C2 C1 H11 . . 109.8
H12 C1 H11 . . 108.2
N1 C2 C1 . . 110.5(7)
N1 C2 H22 . . 109.5
C1 C2 H22 . . 109.5
N1 C2 H21 . . 109.5
C1 C2 H21 . . 109.5
H22 C2 H21 . . 108.1
N1 C3 P2 . . 119.1(6)
N1 C3 H32 . . 107.6
P2 C3 H32 . . 107.6
N1 C3 H31 . . 107.6
P2 C3 H31 . . 107.6
H32 C3 H31 . . 107.0
N1 C4 P1 . . 112.3(5)
N1 C4 H42 . . 109.1
P1 C4 H42 . . 109.1
N1 C4 H41 . . 109.1
P1 C4 H41 . . 109.1
H42 C4 H41 . . 107.9
O8 C5 O10 . . 125.4(8)
O8 C5 C5 . 2_677 117.0(9)
O10 C5 C5 . 2_677 117.5(9)
O7 C6 O9 . . 126.7(7)
O7 C6 C6 . 2_667 118.0(8)
O9 C6 C6 . 2_667 115.2(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Gd1 O5 2_676 2.301(5)
Gd1 O3 . 2.322(5)
Gd1 O2 2_666 2.337(5)
Gd1 O7 . 2.406(5)
Gd1 O8 2_677 2.437(5)
Gd1 O9 2_667 2.452(5)
Gd1 O10 . 2.456(5)
Gd1 O13 . 2.470(7)
P1 O2 . 1.489(5)
P1 O3 . 1.501(5)
P1 O1 . 1.569(6)
P1 C4 . 1.834(8)
P2 O5 . 1.488(5)
P2 O6 . 1.503(7)
P2 O4 . 1.553(6)
P2 C3 . 1.846(8)
N1 C2 . 1.482(11)
N1 C3 . 1.498(9)
N1 C4 . 1.508(10)
N1 H1A . 0.82(8)
O7 C6 . 1.240(9)
O8 C5 . 1.254(9)
O8 Gd1 2_677 2.437(5)
O9 C6 . 1.246(9)
O9 Gd1 2_667 2.452(5)
O10 C5 . 1.257(9)
O1 H1 . 0.8200
O2 Gd1 2_666 2.337(5)
O5 Gd1 2_676 2.301(5)
O4 H4 . 0.8200
O13 H13B . 0.8200
O13 H13A . 0.85(2)
O12 H12B . 0.8595
O12 H12A . 0.8517
O11 H11B . 0.8590
O11 H11A . 0.8447
C1 C1 2_565 1.490(17)
C1 C2 . 1.546(11)
C1 H12 . 0.9700
C1 H11 . 0.9700
C2 H22 . 0.9700
C2 H21 . 0.9700
C3 H32 . 0.9700
C3 H31 . 0.9700
C4 H42 . 0.9700
C4 H41 . 0.9700
C5 C5 2_677 1.517(16)
C6 C6 2_667 1.524(14)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1 O11 2_566 0.82 1.81 2.628(8) 176.5
O13 H13B O11 1_655 0.82 1.94 2.751(10) 168.0
O4 H4 O12 2_676 0.82 1.81 2.602(8) 160.5
O11 H11B O10 2_677 0.86 1.87 2.720(8) 171.8
O12 H12A O6 1_655 0.85 1.92 2.752(10) 164.6
O11 H11A O6 2_576 0.84 1.99 2.805(9) 161.4
