#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/00/2220021.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_2220021
loop_
_publ_author_name
'Liu, Wei'
'Zhang, Lan'
'Hu, Kai'
'Cao, Lixin'
'Su, Ge'
'Zhao, Jingtai'
_publ_section_title
;
 Disodium tricopper(II) tetrakis[selenate(IV)] tetrahydrate
;
_journal_coeditor_code           WM2197
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i78
_journal_paper_doi               10.1107/S160053680803434X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'Na2 Cu3 (Se O3)4 (H2 O)4'
_chemical_formula_structural     'Na2 Cu3 (Se O3)4 (H2 O)4'
_chemical_formula_sum            'Cu3 H8 Na2 O16 Se4'
_chemical_formula_weight         816.50
_chemical_name_systematic
;
disodium tricopper(II) tetrakis[selenate(IV)] tetrahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 92.071(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.2218(5)
_cell_length_b                   8.9863(6)
_cell_length_c                   15.7960(11)
_cell_measurement_reflns_used    986
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.78
_cell_measurement_theta_min      2.58
_cell_volume                     740.74(10)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and DIAMOND (Crystal Impact, 2004)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD'
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6010
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.239
_exptl_absorpt_correction_T_max  0.2501
_exptl_absorpt_correction_T_min  0.2039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    3.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.770
_refine_diff_density_min         -1.020
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0202P)²+3.7977P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0684
_reflns_number_gt                2065
_reflns_number_total             2142
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2197.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2220021
_cod_database_fobs_code          2220021
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Se Se1 0.20254(7) 0.28287(4) 0.09687(2) 0.01090(10) Uani d . 1
Se Se2 -0.79415(7) 0.53958(5) 0.27304(2) 0.01476(11) Uani d . 1
Cu Cu1 0.0000 0.0000 0.0000 0.01381(14) Uani d S 1
Cu Cu2 -0.29891(8) 0.42910(6) 0.17116(3) 0.01266(11) Uani d . 1
O O1 -1.0733(5) 0.4403(4) 0.27181(18) 0.0207(6) Uani d . 1
O O2 -0.0088(5) 0.4276(3) 0.09497(18) 0.0153(5) Uani d . 1
O O3 -0.5831(5) 0.4016(3) 0.24757(18) 0.0165(5) Uani d . 1
O O4 0.1289(6) 0.2058(3) 0.00011(18) 0.0166(5) Uani d . 1
O O5 -0.3653(7) 0.6725(4) 0.1392(2) 0.0209(6) Uani d . 1
O O6 0.2781(6) -0.0756(4) 0.07804(19) 0.0199(6) Uani d . 1
O O7 0.4702(5) 0.3793(3) 0.07309(17) 0.0149(5) Uani d . 1
O O8 -0.7371(6) 0.5600(4) 0.3773(2) 0.0272(7) Uani d . 1
Na Na1 0.7415(3) 0.3619(2) -0.04070(11) 0.0226(4) Uani d . 1
H H1 -0.277(15) 0.707(9) 0.104(5) 0.050 Uiso d . 1
H H2 -0.372(14) 0.748(9) 0.174(5) 0.050 Uiso d . 1
H H4 0.226(15) -0.063(9) 0.131(5) 0.050 Uiso d . 1
H H3 0.437(15) -0.049(9) 0.088(5) 0.050 Uiso d . 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Se Se -0.0929 2.2259 '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
O7 Se1 O2 . . 98.30(14)
O7 Se1 O4 . . 99.75(13)
O2 Se1 O4 . . 99.71(14)
O8 Se2 O1 . . 100.95(16)
O8 Se2 O3 . . 102.54(16)
O1 Se2 O3 . . 100.08(15)
O4 Cu1 O4 . 3 180.00(6)
O4 Cu1 O6 . . 94.50(13)
O4 Cu1 O6 3 . 85.50(13)
O4 Cu1 O6 . 3 85.50(13)
O4 Cu1 O6 3 3 94.50(13)
O6 Cu1 O6 . 3 180.00(14)
O1 Cu2 O3 1_655 . 87.30(12)
O1 Cu2 O2 1_655 . 92.48(12)
O3 Cu2 O2 . . 172.34(13)
O1 Cu2 O7 1_655 1_455 169.80(14)
O3 Cu2 O7 . 1_455 90.00(12)
O2 Cu2 O7 . 1_455 88.88(11)
O1 Cu2 O5 1_655 . 102.39(14)
O3 Cu2 O5 . . 98.36(13)
O2 Cu2 O5 . . 89.17(12)
O7 Cu2 O5 1_455 . 87.73(12)
Se2 O1 Cu2 . 1_455 121.82(17)
Se1 O2 Cu2 . . 120.42(16)
Se1 O2 Na1 . 3_665 102.26(13)
Cu2 O2 Na1 . 3_665 130.61(15)
Se1 O2 Na1 . 1_455 98.62(14)
Cu2 O2 Na1 . 1_455 97.75(12)
Na1 O2 Na1 3_665 1_455 99.28(11)
Se2 O3 Cu2 . . 124.02(17)
Se1 O4 Cu1 . . 116.58(15)
Se1 O4 Na1 . 1_455 98.94(14)
Cu1 O4 Na1 . 1_455 104.54(13)
Cu2 O5 Na1 . 3_565 97.49(13)
Cu2 O5 H1 . . 116(6)
Na1 O5 H1 3_565 . 94(5)
Cu2 O5 H2 . . 129(5)
Na1 O5 H2 3_565 . 116(5)
H1 O5 H2 . . 100(7)
Cu1 O6 Na1 . 3_655 99.94(13)
Cu1 O6 H4 . . 107(5)
Na1 O6 H4 3_655 . 109(5)
Cu1 O6 H3 . . 133(5)
Na1 O6 H3 3_655 . 110(5)
H4 O6 H3 . . 97(7)
Se1 O7 Cu2 . 1_655 115.16(15)
Se1 O7 Na1 . . 131.60(16)
Cu2 O7 Na1 1_655 . 104.37(12)
Se1 O7 Na1 . 3_665 98.71(13)
Cu2 O7 Na1 1_655 3_665 101.13(12)
Na1 O7 Na1 . 3_665 99.95(12)
O7 Na1 O5 . 3_565 90.14(12)
O7 Na1 O2 . 3_665 124.83(13)
O5 Na1 O2 3_565 3_665 108.41(12)
O7 Na1 O4 . 1_655 110.09(12)
O5 Na1 O4 3_565 1_655 134.38(13)
O2 Na1 O4 3_665 1_655 93.18(11)
O7 Na1 O2 . 1_655 69.01(10)
O5 Na1 O2 3_565 1_655 158.39(13)
O2 Na1 O2 3_665 1_655 80.72(11)
O4 Na1 O2 1_655 1_655 62.06(10)
O7 Na1 O7 . 3_665 80.06(12)
O5 Na1 O7 3_565 3_665 70.66(11)
O2 Na1 O7 3_665 3_665 60.11(10)
O4 Na1 O7 1_655 3_665 150.69(12)
O2 Na1 O7 1_655 3_665 99.14(11)
O7 Na1 O6 . 3_655 102.55(12)
O5 Na1 O6 3_565 3_655 73.44(11)
O2 Na1 O6 3_665 3_655 132.30(12)
O4 Na1 O6 1_655 3_655 62.63(11)
O2 Na1 O6 1_655 3_655 115.47(12)
O7 Na1 O6 3_665 3_655 144.02(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
Se1 O7 . 1.698(3) y
Se1 O2 . 1.705(3) y
Se1 O4 . 1.709(3) y
Se2 O8 . 1.673(3) y
Se2 O1 . 1.708(3) y
Se2 O3 . 1.717(3) y
Cu1 O4 . 1.968(3) y
Cu1 O4 3 1.968(3) ?
Cu1 O6 . 1.990(3) y
Cu1 O6 3 1.990(3) ?
Cu1 O8 2_445 2.475(3) ?
Cu1 O8 2_445 2.475(3) y
Cu2 O1 1_655 1.947(3) y
Cu2 O3 . 1.962(3) y
Cu2 O2 . 1.968(3) y
Cu2 O7 1_455 1.980(3) y
Cu2 O5 . 2.268(3) y
Na1 O7 . 2.333(4) ?
Na1 O5 3_565 2.482(4) ?
Na1 O2 3_665 2.519(4) ?
Na1 O4 1_655 2.526(4) ?
Na1 O2 1_655 2.537(3) ?
Na1 O7 3_665 2.618(4) ?
Na1 O6 3_655 2.641(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
O5 H1 O4 3_565 0.80(8) 2.00(8) 2.786(4) 168(7)
O5 H2 O3 2_455 0.87(8) 1.88(8) 2.746(4) 174(7)
O6 H3 O8 2_545 0.87(8) 1.91(8) 2.758(5) 163(7)
O6 H4 O1 2_445 0.89(8) 1.76(8) 2.641(4) 169(8)
