#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/94/2209414.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_2209414
loop_
_publ_author_name
'Wen-Zhi Zhang'
_publ_section_title
Poly[diaqua-μ₄-benzene-1,4-dicarboxylato-di-μ₂-benzene-1,4-dicarboxylato-bis(N,N'-dimethylformamide)digadolinium(III)]
_journal_coeditor_code           BT2107
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1600
_journal_page_last               m1602
_journal_paper_doi               10.1107/S1600536806022884
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Gd2 (C8 H4 O4)3 (C3 H7 N O)2 (H2 O)2]'
_chemical_formula_moiety         'C30 H30 Gd2 N2 O16'
_chemical_formula_sum            'C30 H30 Gd2 N2 O16'
_chemical_formula_weight         989.06
_chemical_name_systematic
;Poly[diaqua-μ₄-benzene-1,4-dicarboxylato-di-μ₂-benzene-1,4-dicarboxylato-
bis(N,N'-dimethylformamide)digadolinium(III)]
;
_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           SHELXL-97
_cell_angle_alpha                65.26(3)
_cell_angle_beta                 71.76(3)
_cell_angle_gamma                78.68(3)
_cell_formula_units_Z            1
_cell_length_a                   8.6066(17)
_cell_length_b                   10.156(2)
_cell_length_c                   11.161(2)
_cell_measurement_reflns_used    7950
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.02
_cell_volume                     839.1(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotor target'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8319
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.995
_exptl_absorpt_correction_T_max  0.316
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.659
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.021P)²+0.6587P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0423
_reflns_number_gt                3626
_reflns_number_total             3806
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt2107.cif
_cod_data_source_block           I
_cod_database_code               2209414
_cod_database_fobs_code          2209414
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
C C1 0.0684(3) 0.2348(2) 0.5526(2) 0.0207(4) Uani d . 1
C C2 0.0326(3) 0.1144(2) 0.5236(2) 0.0207(4) Uani d . 1
C C3 0.0428(3) 0.1312(3) 0.3915(3) 0.0266(5) Uani d . 1
H H3 0.0713 0.2186 0.3189 0.032 Uiso calc R 1
C C4 0.0100(3) 0.0164(3) 0.3687(3) 0.0271(5) Uani d . 1
H H4 0.0167 0.0274 0.2803 0.033 Uiso calc R 1
C C5 0.3254(3) 0.2320(2) 0.8199(2) 0.0224(5) Uani d . 1
C C6 0.4174(3) 0.1110(2) 0.9111(2) 0.0230(5) Uani d . 1
C C7 0.5801(3) 0.0691(3) 0.8640(3) 0.0327(6) Uani d . 1
H H7 0.6347 0.1151 0.7727 0.039 Uiso calc R 1
C C8 0.3380(3) 0.0411(3) 1.0482(3) 0.0340(6) Uani d . 1
H H8 0.2287 0.0688 1.0811 0.041 Uiso calc R 1
C C9 -0.1789(3) 0.4611(2) 0.8309(2) 0.0211(4) Uani d . 1
C C10 -0.3452(3) 0.4823(3) 0.9176(2) 0.0225(5) Uani d . 1
C C11 -0.4747(3) 0.4133(3) 0.9270(3) 0.0297(5) Uani d . 1
H H11 -0.4575 0.3549 0.8777 0.036 Uiso calc R 1
C C12 -0.3704(3) 0.5698(3) 0.9910(3) 0.0284(5) Uani d . 1
H H12 -0.2840 0.6166 0.9852 0.034 Uiso calc R 1
C C13 0.2424(5) 0.6720(3) 0.7523(4) 0.0443(8) Uani d . 1
H H13 0.1506 0.6525 0.8266 0.053 Uiso calc R 1
C C14 0.4844(9) 0.7975(7) 0.6216(7) 0.126(3) Uani d . 1
H H14A 0.5395 0.8720 0.6198 0.189 Uiso calc R 1
H H14B 0.4566 0.8284 0.5364 0.189 Uiso calc R 1
H H14C 0.5553 0.7097 0.6350 0.189 Uiso calc R 1
C C15 0.2894(9) 0.8514(5) 0.8222(7) 0.121(3) Uani d . 1
H H15A 0.3697 0.9192 0.7943 0.182 Uiso calc R 1
H H15B 0.2836 0.7846 0.9146 0.182 Uiso calc R 1
H H15C 0.1841 0.9032 0.8166 0.182 Uiso calc R 1
N N1 0.3361(5) 0.7709(3) 0.7323(4) 0.0669(11) Uani d . 1
O O1 0.0362(2) 0.36646(17) 0.48056(17) 0.0233(3) Uani d . 1
O O2 0.1311(3) 0.20219(19) 0.6491(2) 0.0353(5) Uani d . 1
O O1W 0.3181(3) 0.5427(3) 0.4320(2) 0.0378(5) Uani d . 1
O O3 0.3978(2) 0.29960(19) 0.69548(18) 0.0277(4) Uani d . 1
O O4 0.1783(2) 0.2650(2) 0.86895(18) 0.0304(4) Uani d . 1
O O5 -0.1569(2) 0.38106(18) 0.76416(17) 0.0238(3) Uani d . 1
O O6 -0.0631(2) 0.52337(19) 0.82501(18) 0.0263(4) Uani d . 1
O O7 0.2694(3) 0.6039(2) 0.6784(2) 0.0381(5) Uani d . 1
Gd Gd1 0.131860(13) 0.439754(11) 0.653288(11) 0.01689(4) Uani d . 1
H HW11 0.394(4) 0.580(3) 0.405(3) 0.025 Uiso d . 1
H HW12 0.287(4) 0.562(3) 0.374(3) 0.025 Uiso 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'
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
_geom_angle_publ_flag
O2 C1 O1 . . 121.0(2) ?
O2 C1 C2 . . 118.3(2) ?
O1 C1 C2 . . 120.7(2) ?
O2 C1 Gd1 . . 54.07(12) ?
O1 C1 Gd1 . . 67.12(12) ?
C2 C1 Gd1 . . 171.22(16) ?
C4 C2 C3 2_556 . 119.9(2) ?
C4 C2 C1 2_556 . 118.9(2) ?
C3 C2 C1 . . 121.2(2) ?
C2 C3 C4 . . 119.5(2) ?
C2 C3 H3 . . 120.3 ?
C4 C3 H3 . . 120.3 ?
C2 C4 C3 2_556 . 120.6(2) ?
C2 C4 H4 2_556 . 119.7 ?
C3 C4 H4 . . 119.7 ?
O4 C5 O3 . . 121.4(2) ?
O4 C5 C6 . . 118.9(2) ?
O3 C5 C6 . . 119.8(2) ?
O4 C5 Gd1 . . 58.63(12) ?
O3 C5 Gd1 . . 63.01(12) ?
C6 C5 Gd1 . . 174.47(16) ?
C7 C6 C8 . . 118.9(2) ?
C7 C6 C5 . . 122.0(2) ?
C8 C6 C5 . . 119.1(2) ?
C6 C7 C8 . 2_657 120.4(2) ?
C6 C7 H7 . . 119.8 ?
C8 C7 H7 2_657 . 119.8 ?
C7 C8 C6 2_657 . 120.7(3) ?
C7 C8 H8 2_657 . 119.6 ?
C6 C8 H8 . . 119.6 ?
O6 C9 O5 . . 121.2(2) ?
O6 C9 C10 . . 119.1(2) ?
O5 C9 C10 . . 119.7(2) ?
O6 C9 Gd1 . . 60.18(12) ?
O5 C9 Gd1 . . 61.17(12) ?
C10 C9 Gd1 . . 176.09(16) ?
C11 C10 C12 . . 119.7(2) ?
C11 C10 C9 . . 120.2(2) ?
C12 C10 C9 . . 120.1(2) ?
C10 C11 C12 . 2_467 120.8(2) ?
C10 C11 H11 . . 119.6 ?
C12 C11 H11 2_467 . 119.6 ?
C11 C12 C10 2_467 . 119.4(2) ?
C11 C12 H12 2_467 . 120.3 ?
C10 C12 H12 . . 120.3 ?
O7 C13 N1 . . 123.7(4) ?
O7 C13 H13 . . 118.2 ?
N1 C13 H13 . . 118.2 ?
N1 C14 H14A . . 109.5 ?
N1 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
N1 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
N1 C15 H15A . . 109.5 ?
N1 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
N1 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
C13 N1 C14 . . 119.1(4) ?
C13 N1 C15 . . 119.6(5) ?
C14 N1 C15 . . 121.3(4) ?
C1 O1 Gd1 . 2_566 152.36(16) ?
C1 O1 Gd1 . . 87.44(14) ?
Gd1 O1 Gd1 2_566 . 113.38(6) ?
C1 O2 Gd1 . . 101.43(14) ?
Gd1 O1W HW11 . . 136(3) ?
Gd1 O1W HW12 . . 117(3) ?
HW11 O1W HW12 . . 104(3) ?
C5 O3 Gd1 . . 90.21(15) ?
C5 O4 Gd1 . . 95.14(15) ?
C9 O5 Gd1 . . 92.10(14) ?
C9 O6 Gd1 . . 93.47(14) ?
C13 O7 Gd1 . . 137.2(2) ?
O7 Gd1 O1W . . 76.41(8) y
O7 Gd1 O4 . . 86.94(8) y
O1W Gd1 O4 . . 131.44(7) y
O7 Gd1 O2 . . 148.78(7) y
O1W Gd1 O2 . . 97.10(9) y
O4 Gd1 O2 . . 74.52(7) y
O7 Gd1 O1 . 2_566 93.53(7) ?
O1W Gd1 O1 . 2_566 75.90(7) ?
O4 Gd1 O1 . 2_566 151.47(6) ?
O2 Gd1 O1 . 2_566 114.76(6) ?
O7 Gd1 O6 . . 73.86(7) y
O1W Gd1 O6 . . 138.23(8) y
O4 Gd1 O6 . . 75.39(7) y
O2 Gd1 O6 . . 123.21(7) y
O1 Gd1 O6 2_566 . 77.36(6) ?
O7 Gd1 O5 . . 126.74(7) y
O1W Gd1 O5 . . 141.71(7) y
O4 Gd1 O5 . . 84.01(7) y
O2 Gd1 O5 . . 76.82(7) y
O1 Gd1 O5 2_566 . 72.89(7) ?
O6 Gd1 O5 . . 53.04(6) y
O7 Gd1 O3 . . 76.20(7) y
O1W Gd1 O3 . . 78.70(7) y
O4 Gd1 O3 . . 52.93(7) y
O2 Gd1 O3 . . 72.58(7) y
O1 Gd1 O3 2_566 . 154.23(6) ?
O6 Gd1 O3 . . 120.70(6) y
O5 Gd1 O3 . . 132.12(6) y
O7 Gd1 O1 . . 147.14(7) y
O1W Gd1 O1 . . 73.51(7) y
O4 Gd1 O1 . . 123.21(6) y
O2 Gd1 O1 . . 49.90(6) y
O1 Gd1 O1 2_566 . 66.62(6) ?
O6 Gd1 O1 . . 122.76(6) y
O5 Gd1 O1 . . 74.09(6) y
O3 Gd1 O1 . . 110.02(6) y
O7 Gd1 C9 . . 100.03(8) ?
O1W Gd1 C9 . . 147.76(8) ?
O4 Gd1 C9 . . 79.48(7) ?
O2 Gd1 C9 . . 100.94(8) ?
O1 Gd1 C9 2_566 . 72.34(7) ?
O6 Gd1 C9 . . 26.35(6) ?
O5 Gd1 C9 . . 26.73(6) ?
O3 Gd1 C9 . . 132.25(6) ?
O1 Gd1 C9 . . 98.36(6) ?
O7 Gd1 C5 . . 82.13(7) ?
O1W Gd1 C5 . . 105.48(8) ?
O4 Gd1 C5 . . 26.23(7) ?
O2 Gd1 C5 . . 70.08(7) ?
O1 Gd1 C5 2_566 . 174.92(6) ?
O6 Gd1 C5 . . 98.80(7) ?
O5 Gd1 C5 . . 107.58(7) ?
O3 Gd1 C5 . . 26.78(7) ?
O1 Gd1 C5 . . 118.44(6) ?
C9 Gd1 C5 . . 105.71(7) ?
O7 Gd1 C1 . . 160.36(7) ?
O1W Gd1 C1 . . 86.16(8) ?
O4 Gd1 C1 . . 98.20(7) ?
O2 Gd1 C1 . . 24.50(6) ?
O1 Gd1 C1 2_566 . 90.86(6) ?
O6 Gd1 C1 . . 125.76(6) ?
O5 Gd1 C1 . . 72.81(7) ?
O3 Gd1 C1 . . 91.74(7) ?
O1 Gd1 C1 . . 25.44(6) ?
C9 Gd1 C1 . . 99.54(7) ?
C5 Gd1 C1 . . 94.10(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
C1 O2 . 1.247(3) ?
C1 O1 . 1.267(3) ?
C1 C2 . 1.496(3) ?
C1 Gd1 . 2.947(2) ?
C2 C4 2_556 1.387(3) ?
C2 C3 . 1.387(3) ?
C3 C4 . 1.388(3) ?
C3 H3 . 0.9300 ?
C4 C2 2_556 1.387(3) ?
C4 H4 . 0.9300 ?
C5 O4 . 1.252(3) ?
C5 O3 . 1.271(3) ?
C5 C6 . 1.499(3) ?
C5 Gd1 . 2.822(3) ?
C6 C7 . 1.383(4) ?
C6 C8 . 1.392(4) ?
C7 C8 2_657 1.384(4) ?
C7 H7 . 0.9300 ?
C8 C7 2_657 1.384(4) ?
C8 H8 . 0.9300 ?
C9 O6 . 1.253(3) ?
C9 O5 . 1.268(3) ?
C9 C10 . 1.490(3) ?
C9 Gd1 . 2.818(3) ?
C10 C11 . 1.384(4) ?
C10 C12 . 1.388(3) ?
C11 C12 2_467 1.387(4) ?
C11 H11 . 0.9300 ?
C12 C11 2_467 1.387(4) ?
C12 H12 . 0.9300 ?
C13 O7 . 1.228(4) ?
C13 N1 . 1.314(4) ?
C13 H13 . 0.9300 ?
C14 N1 . 1.448(8) ?
C14 H14A . 0.9600 ?
C14 H14B . 0.9600 ?
C14 H14C . 0.9600 ?
C15 N1 . 1.463(6) ?
C15 H15A . 0.9600 ?
C15 H15B . 0.9600 ?
C15 H15C . 0.9600 ?
O1 Gd1 2_566 2.4436(19) ?
O1 Gd1 . 2.7175(18) y
O2 Gd1 . 2.4343(18) y
O1W Gd1 . 2.404(2) y
O1W HW11 . 0.73(3) ?
O1W HW12 . 0.72(3) ?
O3 Gd1 . 2.5143(19) y
O4 Gd1 . 2.4189(19) y
O5 Gd1 . 2.4703(19) y
O6 Gd1 . 2.4493(19) y
O7 Gd1 . 2.3729(19) y
Gd1 O1 2_566 2.4436(19) ?
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
O1W HW11 O3 2_666 0.73(3) 2.10(3) 2.832(3) 173(3)
O1W HW12 O5 2_566 0.72(3) 2.01(3) 2.717(3) 169(3)
