#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006874.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_2006874
loop_
_publ_author_name
'Barnes, J. C.'
'Weakley, T. J. R.'
_publ_section_title
;
 Disodium Bis(malonato)cuprate(II) Dihydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9700026
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          'Na2 [Cu(C3 H2 O4)2] , 2H2 O'
_chemical_formula_moiety         'Na2,  C6 H4 Cu1 O8 , 2(H2 O)'
_chemical_formula_sum            'C6 H8 Cu Na2 O10'
_chemical_formula_weight         349.6
_chemical_name_systematic
;
Sodium bis(malonato)cuprate(II) dihydrate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_method           'TEXRAY.INF file & SHELXL'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8140(10)
_cell_length_b                   9.497(2)
_cell_length_c                   16.374(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.6
_cell_measurement_theta_min      14.1
_cell_volume                     1059.6(3)
_computing_cell_refinement       'CAD4/PC (Enraf-Nonius, 1993)'
_computing_data_collection       'CAD4/PC (Enraf-Nonius, 1993)'
_computing_data_reduction        'TEXSAN (Molecular Structure Corp., 1989)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.2
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1274
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        -1.40
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.145
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.525
_exptl_absorpt_correction_type   'azimuthal scans'
_exptl_absorpt_process_details   'North, Phillips & Mathews (1968)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.199
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.949
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+2.4439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_ref         0.1425
_reflns_number_gt                923
_reflns_number_observed          950
_reflns_number_total             1274
_reflns_observed_criterion       1.00\s(I)
_reflns_threshold_expression     >2sigma(I)
_[local]_cod_data_source_file    qb0022.cif
_[local]_cod_data_source_block   jcb18
_[local]_cod_cif_authors_sg_H-M  'P b c a    '
_[local]_cod_chemical_formula_sum_orig 'C6 H8 Cu1 Na2 O10'
_cod_original_cell_volume        1059.6(6)
_cod_database_code               2006874
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'1/2+x,1/2-y,   -z'
'   -x,1/2+y,1/2-z'
'1/2-x,   -y,1/2+z'
'   -x,   -y,   -z'
'1/2-x,1/2+y,   +z'
'   +x,1/2-y,1/2+z'
'1/2+x,   +y,1/2-z'
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_type_symbol
Cu1 0.0000 0.5000 0.0000 0.0170(2) Uani d S 1 Cu
Na2 0.0001(2) 0.36222(18) 0.20012(11) 0.0243(4) Uani d . 1 Na
C1 -0.1286(6) 0.6887(4) 0.1262(2) 0.0177(7) Uani d . 1 C
O2 -0.2000(5) 0.7204(3) 0.19476(18) 0.0281(7) Uani d . 1 O
O3 -0.1077(4) 0.5621(3) 0.10373(16) 0.0200(6) Uani d . 1 O
C4 -0.0638(6) 0.8084(4) 0.0725(2) 0.0183(8) Uani d . 1 C
H41 -0.104(7) 0.896(5) 0.093(3) 0.027 Uiso d . 1 H
H42 0.076(8) 0.814(5) 0.081(3) 0.027 Uiso d . 1 H
C5 -0.1009(6) 0.7936(4) -0.0182(2) 0.0183(8) Uani d . 1 C
O6 -0.1730(5) 0.8951(3) -0.05414(18) 0.0260(7) Uani d . 1 O
O7 -0.0526(4) 0.6789(3) -0.05416(16) 0.0193(6) Uani d . 1 O
O8 -0.2029(5) 0.4898(3) 0.2925(2) 0.0245(7) Uani d . 1 O
H81 -0.205(9) 0.521(6) 0.337(4) 0.037 Uiso d . 1 H
H82 -0.217(9) 0.562(6) 0.267(3) 0.037 Uiso d . 1 H
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
Cu1 0.0218(4) 0.0142(4) 0.0150(4) 0.0032(2) 0.0031(3) -0.0004(2)
Na2 0.0214(8) 0.0249(8) 0.0266(9) -0.0039(6) 0.0011(7) -0.0012(7)
C1 0.0142(16) 0.0204(18) 0.0185(17) 0.0012(15) -0.0021(14) 0.0000(14)
O2 0.0410(18) 0.0227(14) 0.0205(15) 0.0061(13) 0.0081(14) -0.0009(12)
O3 0.0239(14) 0.0168(13) 0.0193(13) -0.0003(11) 0.0046(11) -0.0018(11)
C4 0.0167(17) 0.0153(17) 0.0229(19) 0.0010(14) 0.0006(15) -0.0017(15)
C5 0.0155(18) 0.0164(17) 0.0229(19) -0.0037(14) 0.0030(16) 0.0036(14)
O6 0.0321(16) 0.0196(14) 0.0264(15) 0.0062(12) -0.0001(13) 0.0072(12)
O7 0.0251(14) 0.0153(12) 0.0176(13) 0.0019(11) -0.0009(11) -0.0013(10)
O8 0.0314(18) 0.0230(15) 0.0192(15) -0.0010(13) 0.0029(13) 0.0014(12)
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'
Cu Cu 0.3201 1.2651 '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'
O O 0.0106 0.0060 '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
O3 Cu1 O3 . 5_565 180.0 ?
O3 Cu1 O7 . 5_565 86.35(12) ?
O3 Cu1 O7 5_565 5_565 93.65(12) ?
O3 Cu1 O7 . . 93.65(12) yes
O3 Cu1 O7 5_565 . 86.35(12) ?
O7 Cu1 O7 5_565 . 180.0 ?
O3 Cu1 Na2 . 5_565 134.39(9) ?
O3 Cu1 Na2 5_565 5_565 45.61(9) ?
O7 Cu1 Na2 5_565 5_565 138.21(8) ?
O7 Cu1 Na2 . 5_565 41.79(8) ?
O3 Cu1 Na2 . . 45.61(9) ?
O3 Cu1 Na2 5_565 . 134.39(9) ?
O7 Cu1 Na2 5_565 . 41.79(8) ?
O7 Cu1 Na2 . . 138.21(8) ?
Na2 Cu1 Na2 5_565 . 180.0 ?
O8 Na2 O8 8_656 . 101.79(12) yes
O8 Na2 O7 8_656 5_565 90.39(12) yes
O8 Na2 O7 . 5_565 141.84(13) yes
O8 Na2 O2 8_656 6 177.40(14) yes
O8 Na2 O2 . 6 79.48(12) ?
O7 Na2 O2 5_565 6 89.95(11) ?
O8 Na2 O2 8_656 3_545 77.34(12) yes
O8 Na2 O2 . 3_545 98.56(12) yes
O7 Na2 O2 5_565 3_545 119.46(12) yes
O2 Na2 O2 6 3_545 100.25(12) yes
O8 Na2 O3 8_656 . 84.13(11) ?
O8 Na2 O3 . . 81.28(11) yes
O7 Na2 O3 5_565 . 63.97(10) yes
O2 Na2 O3 6 . 98.33(11) ?
O2 Na2 O3 3_545 . 161.06(12) ?
O8 Na2 Cu1 8_656 . 81.81(9) ?
O8 Na2 Cu1 . . 113.65(10) ?
O7 Na2 Cu1 5_565 . 32.07(7) ?
O2 Na2 Cu1 6 . 99.81(9) ?
O2 Na2 Cu1 3_545 . 144.57(9) ?
O3 Na2 Cu1 . . 32.60(6) ?
O8 Na2 Na2 8_656 8_656 37.37(8) ?
O8 Na2 Na2 . 8_656 104.44(11) ?
O7 Na2 Na2 5_565 8_656 106.88(9) ?
O2 Na2 Na2 6 8_656 140.19(9) ?
O2 Na2 Na2 3_545 8_656 40.01(8) ?
O3 Na2 Na2 . 8_656 121.48(8) ?
Cu1 Na2 Na2 . 8_656 113.69(5) ?
O8 Na2 Na2 8_656 8_556 138.63(10) ?
O8 Na2 Na2 . 8_556 37.01(9) ?
O7 Na2 Na2 5_565 8_556 123.63(10) ?
O2 Na2 Na2 6 8_556 42.51(8) ?
O2 Na2 Na2 3_545 8_556 100.83(10) ?
O3 Na2 Na2 . 8_556 90.43(7) ?
Cu1 Na2 Na2 . 8_556 113.66(5) ?
Na2 Na2 Na2 8_656 8_556 128.77(10) ?
O2 C1 O3 . . 122.0(4) yes
O2 C1 C4 . . 117.0(3) yes
O3 C1 C4 . . 121.0(4) yes
C1 O2 Na2 . 6_565 119.1(3) ?
C1 O2 Na2 . 3 121.1(3) ?
Na2 O2 Na2 6_565 3 97.48(11) ?
C1 O3 Cu1 . . 125.8(3) ?
C1 O3 Na2 . . 123.6(2) ?
Cu1 O3 Na2 . . 101.78(12) ?
C1 C4 C5 . . 117.1(3) yes
O6 C5 O7 . . 123.2(4) yes
O6 C5 C4 . . 117.6(4) yes
O7 C5 C4 . . 119.2(3) yes
C5 O7 Cu1 . . 125.3(3) ?
C5 O7 Na2 . 5_565 128.5(3) ?
Cu1 O7 Na2 . 5_565 106.14(12) ?
Na2 O8 Na2 8_556 . 105.62(14) ?
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
Cu1 O3 . 1.942(3) yes
Cu1 O3 5_565 1.942(3) ?
Cu1 O7 5_565 1.950(3) ?
Cu1 O7 . 1.950(3) yes
Cu1 Na2 5_565 3.5284(18) ?
Cu1 Na2 . 3.5284(18) ?
Na2 O8 8_555 2.361(4) ?
Na2 O8 . 2.381(4) yes
Na2 O7 5_565 2.448(3) yes
Na2 O2 6_445 2.450(4) yes
Na2 O2 3_545 2.575(4) yes
Na2 O3 . 2.576(3) yes
Na2 Na2 8_656 3.7783(16) ?
Na2 Na2 8_556 3.7783(16) ?
C1 O2 . 1.260(5) yes
C1 O3 . 1.265(5) yes
C1 C4 . 1.504(5) yes
O2 Na2 6_565 2.450(4) ?
O2 Na2 3 2.575(4) ?
C4 C5 . 1.512(6) yes
C5 O6 . 1.232(5) yes
C5 O7 . 1.281(5) yes
O7 Na2 5_565 2.448(3) ?
O8 Na2 8_556 2.361(4) ?
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
O8 H82 O2 . 0.80(6) 1.92(6) 2.713(4) 168(6)
O8 H81 O6 7_565 0.79(7) 1.97(7) 2.746(4) 172(6)