#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:36:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179385 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/82/4328275.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_4328275
loop_
_publ_author_name
'Wassim Maalej'
'Serge Vilminot'
'Gilles André'
'Zakaria Elaoud'
'Tahar Mhiri'
'Mohamedally Kurmoo'
_publ_section_title
;
 Crystal and Magnetic Structures and Magnetic Properties of Selenate
 Containing Natrochalcite, AIMII2(H3O2)(SeO4)2 Where A = Na or K and M =
 Mn, Co, or Ni
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1953
_journal_page_last               1962
_journal_paper_doi               10.1021/ic202273e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'H3 Na Ni2 O10 Se2'
_chemical_formula_weight         461.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 114.5310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8476(4)
_cell_length_b                   6.2451(3)
_cell_length_c                   7.4883(4)
_cell_measurement_temperature    293(2)
_cell_volume                     376.41(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1276
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         4.13
_exptl_absorpt_coefficient_mu    14.773
_exptl_crystal_density_diffrn    4.071
_exptl_crystal_F_000             436
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0077(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0145
_refine_ls_R_factor_gt           0.0142
_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)+(0.0266P)²+0.2254P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0404
_reflns_number_gt                452
_reflns_number_total             460
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202273e_si_003.cif
_cod_data_source_block           nanisesplit
_cod_database_code               4328275
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni Ni 0.2500 0.2500 0.0000 0.00425(14) Uani 1 2 d S
Se Se 0.08629(3) 0.0000 0.29183(4) 0.00407(13) Uani 1 2 d S
O1 O 0.2304(3) 0.0000 0.5121(3) 0.0096(4) Uani 1 2 d S
O2 O 0.1825(2) 0.0000 0.1411(3) 0.0068(4) Uani 1 2 d S
O3 O -0.02978(17) 0.2157(2) 0.2490(2) 0.0068(3) Uani 1 1 d .
OH O 0.3483(2) 0.0000 -0.0821(3) 0.0055(4) Uani 1 2 d S
Na1 Na 0.0000 0.5000 0.5000 0.0120(4) Uani 1 4 d S
H1 H 0.315(5) 0.0000 -0.193(7) 0.017(11) Uiso 1 2 d S
H2 H 0.554(9) 0.0000 0.038(14) 0.02(2) Uiso 0.50 2 d SP
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Se Se -0.0929 2.2259 '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'
Ni Ni 0.3393 1.1124 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
OH Ni OH 180.0 . 7
OH Ni O3 89.47(7) . 8
OH Ni O3 90.53(7) 7 8
OH Ni O3 90.53(7) . 2
OH Ni O3 89.47(7) 7 2
O3 Ni O3 180.0 8 2
OH Ni O2 79.99(6) . .
OH Ni O2 100.01(6) 7 .
O3 Ni O2 88.95(7) 8 .
O3 Ni O2 91.05(7) 2 .
OH Ni O2 100.01(6) . 7
OH Ni O2 79.99(6) 7 7
O3 Ni O2 91.05(7) 8 7
O3 Ni O2 88.95(7) 2 7
O2 Ni O2 180.0 . 7
O1 Se O3 111.37(7) . 6
O1 Se O3 111.37(7) . .
O3 Se O3 110.18(10) 6 .
O1 Se O2 106.41(11) . .
O3 Se O2 108.69(6) 6 .
O3 Se O2 108.69(6) . .
O1 Se Na1 43.32(8) . 3_545
O3 Se Na1 124.60(5) 6 3_545
O3 Se Na1 124.60(5) . 3_545
O2 Se Na1 63.09(7) . 3_545
Se O1 Na1 109.53(11) . 3_545
Se O2 Ni 131.96(4) . .
Se O2 Ni 131.96(4) . 4_545
Ni O2 Ni 95.68(8) . 4_545
Se O2 Na1 86.83(8) . 3_545
Ni O2 Na1 95.45(6) . 3_545
Ni O2 Na1 95.45(6) 4_545 3_545
Se O3 Ni 122.53(8) . 2
Se O3 Na1 124.69(8) . .
Ni O3 Na1 111.49(6) 2 .
Ni OH Ni 102.34(9) 4_545 .
O1 Na1 O1 180.0 7_556 3_455
O1 Na1 O3 76.81(5) 7_556 .
O1 Na1 O3 103.19(5) 3_455 .
O1 Na1 O3 103.19(5) 7_556 5_566
O1 Na1 O3 76.81(5) 3_455 5_566
O3 Na1 O3 179.999(1) . 5_566
O1 Na1 O3 103.19(5) 7_556 2_556
O1 Na1 O3 76.81(5) 3_455 2_556
O3 Na1 O3 90.35(7) . 2_556
O3 Na1 O3 89.65(7) 5_566 2_556
O1 Na1 O3 76.81(5) 7_556 6_565
O1 Na1 O3 103.19(5) 3_455 6_565
O3 Na1 O3 89.65(7) . 6_565
O3 Na1 O3 90.35(7) 5_566 6_565
O3 Na1 O3 180.0 2_556 6_565
O1 Na1 O2 57.23(6) 7_556 7_556
O1 Na1 O2 122.77(6) 3_455 7_556
O3 Na1 O2 116.18(4) . 7_556
O3 Na1 O2 63.82(4) 5_566 7_556
O3 Na1 O2 63.82(4) 2_556 7_556
O3 Na1 O2 116.18(4) 6_565 7_556
O1 Na1 O2 122.77(6) 7_556 3_455
O1 Na1 O2 57.23(6) 3_455 3_455
O3 Na1 O2 63.82(4) . 3_455
O3 Na1 O2 116.18(4) 5_566 3_455
O3 Na1 O2 116.18(4) 2_556 3_455
O3 Na1 O2 63.82(4) 6_565 3_455
O2 Na1 O2 180.0 7_556 3_455
O1 Na1 Se 27.15(5) 7_556 7_556
O1 Na1 Se 152.85(5) 3_455 7_556
O3 Na1 Se 95.94(3) . 7_556
O3 Na1 Se 84.06(3) 5_566 7_556
O3 Na1 Se 84.06(3) 2_556 7_556
O3 Na1 Se 95.94(3) 6_565 7_556
O2 Na1 Se 30.08(4) 7_556 7_556
O2 Na1 Se 149.92(4) 3_455 7_556
O1 Na1 Se 152.85(5) 7_556 3_455
O1 Na1 Se 27.15(5) 3_455 3_455
O3 Na1 Se 84.06(3) . 3_455
O3 Na1 Se 95.94(3) 5_566 3_455
O3 Na1 Se 95.94(3) 2_556 3_455
O3 Na1 Se 84.06(3) 6_565 3_455
O2 Na1 Se 149.92(4) 7_556 3_455
O2 Na1 Se 30.08(4) 3_455 3_455
Se Na1 Se 180.0 7_556 3_455
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni OH 2.0042(12) .
Ni OH 2.0042(12) 7
Ni O3 2.0742(15) 8
Ni O3 2.0742(15) 2
Ni O2 2.1061(13) .
Ni O2 2.1061(13) 7
Se O1 1.613(2) .
Se O3 1.6430(14) 6
Se O3 1.6430(14) .
Se O2 1.6718(19) .
Se Na1 3.3302(3) 3_545
O1 Na1 2.424(2) 3_545
O2 Ni 2.1061(13) 4_545
O2 Na1 2.974(2) 3_545
O3 Ni 2.0742(15) 2
O3 Na1 2.5183(15) .
OH Ni 2.0042(12) 4_545
Na1 O1 2.424(2) 7_556
Na1 O1 2.424(2) 3_455
Na1 O3 2.5183(15) 5_566
Na1 O3 2.5183(15) 2_556
Na1 O3 2.5183(15) 6_565
Na1 O2 2.974(2) 7_556
Na1 O2 2.974(2) 3_455
Na1 Se 3.3301(3) 7_556
Na1 Se 3.3302(3) 3_455
