#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/78/2227845.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_2227845
loop_
_publ_author_name
'Wu, Jiang'
'Zhu, Hong-lin'
_publ_section_title
;
 Poly[[μ₁₀-2,3-bis(carboxymethyl)butanedioato]disodium]
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1419
_journal_paper_doi               10.1107/S1600536810040857
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Na2 (C8 H8 O8)]'
_chemical_formula_moiety         'C8 H8 Na2 O8'
_chemical_formula_sum            'C8 H8 Na2 O8'
_chemical_formula_weight         278.12
_chemical_name_systematic
;
Poly[[μ₁₀-2,3-bis(carboxymethyl)butanedioato]disodium]
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9053(18)
_cell_length_b                   8.6395(17)
_cell_length_c                   12.527(3)
_cell_measurement_reflns_used    7116
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.25
_cell_volume                     963.8(4)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scan'
_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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0123
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8610
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1097
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0658P)²+0.5154P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                1000
_reflns_number_total             1097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ng5044.cif
_cod_data_source_block           I
_cod_original_cell_volume        963.8(3)
_cod_database_code               2227845
_cod_database_fobs_code          2227845
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Na Na 0.91916(8) 0.06655(8) 0.62976(5) 0.0292(2) Uani d . 1 . .
O O1 1.12521(17) 0.21959(14) 0.69249(10) 0.0391(4) Uani d . 1 . .
O O2 1.30500(16) 0.37558(13) 0.75029(10) 0.0325(3) Uani d D 1 . .
C C1 1.19167(19) 0.34236(18) 0.68752(12) 0.0243(3) Uani d . 1 . .
C C2 1.15019(18) 0.46906(17) 0.61037(11) 0.0219(3) Uani d . 1 . .
H H2A 1.2386 0.4963 0.5692 0.026 Uiso calc R 1 . .
H H2B 1.1207 0.5598 0.6508 0.026 Uiso calc R 1 . .
C C3 1.02287(16) 0.42768(14) 0.53277(10) 0.0161(3) Uani d . 1 . .
H H3A 0.9358 0.3927 0.5741 0.019 Uiso calc R 1 . .
C C4 1.07185(16) 0.29671(16) 0.45770(11) 0.0177(3) Uani d . 1 . .
O O3 1.01257(15) 0.16760(12) 0.46431(9) 0.0300(3) Uani d . 1 . .
O O4 1.17325(15) 0.33112(14) 0.39020(10) 0.0300(3) Uani d . 1 . .
H H2C 1.310(4) 0.308(3) 0.7989(19) 0.088(11) Uiso d D 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Na 0.0336(4) 0.0244(4) 0.0296(4) -0.0038(3) 0.0023(3) -0.0031(2)
O1 0.0481(8) 0.0278(7) 0.0415(7) -0.0062(6) -0.0172(6) 0.0104(5)
O2 0.0432(7) 0.0262(6) 0.0282(6) 0.0011(5) -0.0177(5) 0.0041(5)
C1 0.0305(8) 0.0216(7) 0.0208(7) 0.0046(6) -0.0054(6) -0.0007(5)
C2 0.0278(7) 0.0185(7) 0.0194(7) 0.0020(6) -0.0054(6) 0.0003(5)
C3 0.0208(7) 0.0137(6) 0.0138(6) 0.0032(5) 0.0005(5) 0.0002(5)
C4 0.0212(7) 0.0160(6) 0.0159(6) 0.0039(5) -0.0012(5) -0.0008(5)
O3 0.0448(7) 0.0166(5) 0.0286(6) -0.0050(5) 0.0081(5) -0.0041(4)
O4 0.0340(6) 0.0247(6) 0.0314(6) -0.0026(5) 0.0148(5) -0.0082(5)
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'
Na Na 0.0362 0.0249 '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
O4 Na O1 4_456 . 122.39(5) ?
O4 Na O3 4_456 . 95.36(5) ?
O1 Na O3 . . 79.44(5) ?
O4 Na O3 4_456 5_756 119.46(5) ?
O1 Na O3 . 5_756 115.41(6) ?
O3 Na O3 . 5_756 78.24(5) ?
O4 Na O2 4_456 6_557 86.14(5) ?
O1 Na O2 . 6_557 119.22(5) ?
O3 Na O2 . 6_557 156.69(5) ?
O3 Na O2 5_756 6_557 80.80(5) ?
O4 Na O1 4_456 3_756 76.26(5) ?
O1 Na O1 . 3_756 63.76(7) ?
O3 Na O1 . 3_756 127.10(5) ?
O3 Na O1 5_756 3_756 150.95(5) ?
O2 Na O1 6_557 3_756 75.89(5) ?
O4 Na Na 4_456 3_756 119.52(4) ?
O1 Na Na . 3_756 51.20(4) ?
O3 Na Na . 3_756 129.07(5) ?
O3 Na Na 5_756 3_756 109.34(4) ?
O2 Na Na 6_557 3_756 68.03(4) ?
O1 Na Na 3_756 3_756 45.42(3) ?
O4 Na Na 4_456 5_756 112.22(4) ?
O1 Na Na . 5_756 99.22(5) ?
O3 Na Na . 5_756 39.32(3) ?
O3 Na Na 5_756 5_756 38.92(3) ?
O2 Na Na 6_557 5_756 119.06(4) ?
O1 Na Na 3_756 5_756 162.35(5) ?
Na Na Na 3_756 5_756 128.23(4) ?
C1 O1 Na . . 146.90(11) ?
C1 O1 Na . 3_756 123.86(11) ?
Na O1 Na . 3_756 83.38(5) ?
C1 O2 Na . 6_667 146.49(11) ?
C1 O2 H2C . . 109(2) ?
Na O2 H2C 6_667 . 90(2) ?
O1 C1 O2 . . 122.32(14) ?
O1 C1 C2 . . 123.18(14) ?
O2 C1 C2 . . 114.49(14) ?
C1 C2 C3 . . 114.71(13) ?
C1 C2 H2A . . 108.6 ?
C3 C2 H2A . . 108.6 ?
C1 C2 H2B . . 108.6 ?
C3 C2 H2B . . 108.6 ?
H2A C2 H2B . . 107.6 ?
C4 C3 C2 . . 110.47(11) ?
C4 C3 C3 . 5_766 110.16(13) ?
C2 C3 C3 . 5_766 109.98(14) ?
C4 C3 H3A . . 108.7 ?
C2 C3 H3A . . 108.7 ?
C3 C3 H3A 5_766 . 108.7 ?
O3 C4 O4 . . 123.93(13) ?
O3 C4 C3 . . 120.17(12) ?
O4 C4 C3 . . 115.89(12) ?
C4 O3 Na . . 122.30(9) ?
C4 O3 Na . 5_756 127.90(10) ?
Na O3 Na . 5_756 101.76(5) ?
C4 O4 Na . 4_556 144.24(11) ?
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
Na O4 4_456 2.3748(15) ?
Na O1 . 2.3943(15) ?
Na O3 . 2.3978(13) ?
Na O3 5_756 2.4188(13) ?
Na O2 6_557 2.4522(14) ?
Na O1 3_756 2.6196(15) ?
Na Na 3_756 3.3388(14) ?
Na Na 5_756 3.7369(14) ?
O1 C1 . 1.216(2) ?
O1 Na 3_756 2.6196(15) ?
O2 C1 . 1.311(2) ?
O2 Na 6_667 2.4522(14) ?
O2 H2C . 0.843(10) ?
C1 C2 . 1.506(2) ?
C2 C3 . 1.536(2) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 C4 . 1.5346(18) ?
C3 C3 5_766 1.550(2) ?
C3 H3A . 0.9800 ?
C4 O3 . 1.2368(18) ?
C4 O4 . 1.2723(19) ?
O3 Na 5_756 2.4188(13) ?
O4 Na 4_556 2.3748(15) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O2 H2C O4 . . 2_755 0.85(2) 1.67(3) 2.5097(18) 177(2) y
