#\#CIF_1.1
 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2004-01-30 at 11:25:48
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.3
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : ljf108 dreduc sortabs sortav struct
 
 
data_ljf108
 
_audit_creation_date                    2004-01-30T11:25:48-00:00
_audit_creation_method                  'WinGX routine CIF_UPDATE'
_audit_conform_dict_name                cif_core.dic
_audit_conform_dict_version             2.3
_audit_conform_dict_location            ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category                FM
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C6 H13 Na Ni O11, H2 O'
_chemical_formula_sum                   'C6 H15 Na Ni O12'
_chemical_formula_weight                360.86
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  triclinic
_symmetry_space_group_name_H-M          'P -1'
_symmetry_space_group_name_Hall         '-P 1'
_symmetry_Int_Tables_number             2
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
 
_cell_length_a                          7.6298(3)
_cell_length_b                          8.7188(4)
_cell_length_c                          10.4876(4)
_cell_angle_alpha                       111.214(2)
_cell_angle_beta                        103.631(2)
_cell_angle_gamma                       93.052(2)
_cell_volume                            624.64(4)
_cell_formula_units_Z                   2
_cell_measurement_temperature           100(2)
_cell_measurement_reflns_used           3263
_cell_measurement_theta_min             2.19
_cell_measurement_theta_max             30.034
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   green
_exptl_crystal_size_max                 0.2
_exptl_crystal_size_mid                 0.15
_exptl_crystal_size_min                 0.08
_exptl_crystal_density_diffrn           1.919
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    372
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           1.65
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min         0.765
_exptl_absorpt_correction_T_max         0.825
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'Enraf Nonius FR590'
_diffrn_ambient_temperature             100(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_radiation_probe                 x-ray
_diffrn_detector                        'CCD plate'
_diffrn_orient_matrix_type              'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11             -0.55692E-2
_diffrn_orient_matrix_ub_12             -0.04383
_diffrn_orient_matrix_ub_13             -0.103377
_diffrn_orient_matrix_ub_21             0.12077
_diffrn_orient_matrix_ub_22             0.68789E-1
_diffrn_orient_matrix_ub_23             0.226679E-1
_diffrn_orient_matrix_ub_31             0.633033E-1
_diffrn_orient_matrix_ub_32             -0.940544E-1
_diffrn_orient_matrix_ub_33             0.104449E-1
_diffrn_measurement_device              '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type         KappaCCD
_diffrn_measurement_method              'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents         0.0323
_diffrn_reflns_av_unetI/netI            0.0318
_diffrn_reflns_number                   11245
_diffrn_reflns_limit_h_min              -10
_diffrn_reflns_limit_h_max              10
_diffrn_reflns_limit_k_min              -12
_diffrn_reflns_limit_k_max              12
_diffrn_reflns_limit_l_min              -14
_diffrn_reflns_limit_l_max              14
_diffrn_reflns_theta_min                2.62
_diffrn_reflns_theta_max                30.13
_diffrn_reflns_theta_full               30.13
_diffrn_measured_fraction_theta_full
                                        0.987
_diffrn_measured_fraction_theta_max
                                        0.987
_reflns_number_total                    3636
_reflns_number_gt                       3265
_reflns_threshold_expression            >2sigma(I)
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_data_collection              'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement
                                       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
                             'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution           'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1999)'
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0157P)²+0.4337P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          geom
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            none
_refine_ls_number_reflns                3636
_refine_ls_number_parameters            225
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0308
_refine_ls_R_factor_gt                  0.0248
_refine_ls_wR_factor_ref                0.0555
_refine_ls_wR_factor_gt                 0.0537
_refine_ls_goodness_of_fit_ref          1.049
_refine_ls_restrained_S_all             1.049
_refine_ls_shift/su_max                 0.007
_refine_ls_shift/su_mean                0.001
_refine_diff_density_max                0.456
_refine_diff_density_min                -0.492
_refine_diff_density_rms                0.07
 
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
 
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
Ni Ni 0.3393 1.1124 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
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
    _atom_site_disorder_assembly
    _atom_site_disorder_group
Ni1 Ni 0.97444(2) 0.49818(2) 0.748144(17) 0.00679(5) Uani 1 1 d . . .
Na1 Na 1.20207(8) 0.16854(7) 0.75438(6) 0.01005(11) Uani 1 1 d . . .
O2 O 0.76612(13) 0.48410(12) 0.57515(10) 0.00750(18) Uani 1 1 d . . .
O10 O 0.84957(13) 0.40541(12) 0.33589(10) 0.01069(19) Uani 1 1 d . . .
O11 O 0.60318(15) 0.32328(14) 0.15021(11) 0.0160(2) Uani 1 1 d . . .
O21 O 0.97811(13) 0.26365(12) 0.61150(10) 0.00967(19) Uani 1 1 d . . .
O22 O 0.77322(14) 0.04289(12) 0.45660(10) 0.0117(2) Uani 1 1 d . . .
O31 O 0.77723(13) 0.41219(12) 0.81670(10) 0.01005(19) Uani 1 1 d . . .
O32 O 0.51276(14) 0.28393(13) 0.80810(10) 0.01131(19) Uani 1 1 d . . .
O100 O 0.74475(16) 0.09520(14) 0.91240(11) 0.0136(2) Uani 1 1 d . . .
O110 O 1.18094(14) 0.46516(12) 0.89795(10) 0.00919(18) Uani 1 1 d . . .
O120 O 1.28222(15) 0.14375(14) 0.97581(11) 0.0135(2) Uani 1 1 d . . .
O130 O 0.92170(16) -0.03767(14) 0.70260(12) 0.0158(2) Uani 1 1 d . . .
O140 O 0.96085(15) 0.73899(12) 0.86872(11) 0.0116(2) Uani 1 1 d . . .
C1 C 0.57799(18) 0.27039(17) 0.35298(13) 0.0085(2) Uani 1 1 d . . .
H1A H 0.5466 0.1479 0.3034 0.01 Uiso 1 1 calc R . .
H1B H 0.4621 0.3168 0.3493 0.01 Uiso 1 1 calc R . .
C2 C 0.67832(18) 0.31132(16) 0.50937(13) 0.0070(2) Uani 1 1 d . . .
C3 C 0.54143(18) 0.29218(16) 0.59031(13) 0.0085(2) Uani 1 1 d . . .
H3A H 0.478 0.1758 0.5444 0.01 Uiso 1 1 calc R . .
H3B H 0.4485 0.3646 0.5783 0.01 Uiso 1 1 calc R . .
C10 C 0.68373(19) 0.33578(16) 0.27202(14) 0.0090(2) Uani 1 1 d . . .
C21 C 0.82192(18) 0.19508(16) 0.52457(13) 0.0078(2) Uani 1 1 d . . .
C31 C 0.61586(19) 0.33251(16) 0.74970(14) 0.0083(2) Uani 1 1 d . . .
H2 H 0.817(3) 0.492(2) 0.516(2) 0.018(5) Uiso 1 1 d . . .
H100 H 0.783(3) 0.058(3) 0.839(2) 0.035(6) Uiso 1 1 d . . .
H101 H 0.668(4) 0.155(3) 0.891(3) 0.043(7) Uiso 1 1 d . . .
H110 H 1.182(3) 0.498(3) 0.983(2) 0.029(6) Uiso 1 1 d . . .
H111 H 1.274(3) 0.524(3) 0.900(2) 0.026(5) Uiso 1 1 d . . .
H120 H 1.281(3) 0.064(3) 0.996(2) 0.028(6) Uiso 1 1 d . . .
H121 H 1.377(3) 0.205(3) 1.022(2) 0.030(6) Uiso 1 1 d . . .
H130 H 0.890(3) -0.050(3) 0.624(3) 0.034(6) Uiso 1 1 d . . .
H131 H 0.939(3) -0.125(3) 0.710(2) 0.032(6) Uiso 1 1 d . . .
H140 H 0.881(3) 0.762(3) 0.911(2) 0.037(6) Uiso 1 1 d . . .
H141 H 1.059(4) 0.790(3) 0.934(3) 0.049(8) Uiso 1 1 d . . .
 
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_distance
    _geom_bond_site_symmetry_2
    _geom_bond_publ_flag
Ni1 O31 2.0305(10) . ?
Ni1 O21 2.0348(10) . ?
Ni1 O140 2.0449(10) . ?
Ni1 O110 2.0598(10) . ?
Ni1 O10 2.0639(10) 2_766 ?
Ni1 O2 2.0716(10) . ?
Ni1 Na1 3.4489(6) . ?
Na1 O120 2.3498(12) . ?
Na1 O22 2.3689(11) 2_756 ?
Na1 O32 2.3781(12) 1_655 ?
Na1 O21 2.3866(11) . ?
Na1 O110 2.5144(11) . ?
Na1 O130 2.5377(13) . ?
O2 C2 1.4549(15) . ?
O2 H2 0.83(2) . ?
O10 C10 1.2817(17) . ?
O10 Ni1 2.0639(10) 2_766 ?
O11 C10 1.2425(17) . ?
O21 C21 1.2753(16) . ?
O22 C21 1.2430(16) . ?
O22 Na1 2.3689(11) 2_756 ?
O31 C31 1.2807(17) . ?
O32 C31 1.2461(16) . ?
O32 Na1 2.3781(12) 1_455 ?
O100 H100 0.84(2) . ?
O100 H101 0.85(3) . ?
O110 H110 0.83(2) . ?
O110 H111 0.85(2) . ?
O120 H120 0.79(2) . ?
O120 H121 0.80(2) . ?
O130 H130 0.77(2) . ?
O130 H131 0.81(2) . ?
O140 H140 0.83(3) . ?
O140 H141 0.85(3) . ?
C1 C10 1.5235(18) . ?
C1 C2 1.5359(18) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 C3 1.5301(18) . ?
C2 C21 1.5510(19) . ?
C3 C31 1.5317(18) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
 
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
    _geom_angle_publ_flag
O31 Ni1 O21 90.99(4) . . ?
O31 Ni1 O140 91.13(4) . . ?
O21 Ni1 O140 174.52(4) . . ?
O31 Ni1 O110 92.66(4) . . ?
O21 Ni1 O110 88.79(4) . . ?
O140 Ni1 O110 96.16(4) . . ?
O31 Ni1 O10 173.17(4) . 2_766 ?
O21 Ni1 O10 90.41(4) . 2_766 ?
O140 Ni1 O10 86.89(4) . 2_766 ?
O110 Ni1 O10 94.05(4) . 2_766 ?
O31 Ni1 O2 86.30(4) . . ?
O21 Ni1 O2 80.40(4) . . ?
O140 Ni1 O2 94.69(4) . . ?
O110 Ni1 O2 169.12(4) . . ?
O10 Ni1 O2 87.35(4) 2_766 . ?
O31 Ni1 Na1 90.64(3) . . ?
O21 Ni1 Na1 42.55(3) . . ?
O140 Ni1 Na1 142.46(3) . . ?
O110 Ni1 Na1 46.30(3) . . ?
O10 Ni1 Na1 94.91(3) 2_766 . ?
O2 Ni1 Na1 122.84(3) . . ?
O120 Na1 O22 122.26(4) . 2_756 ?
O120 Na1 O32 86.36(4) . 1_655 ?
O22 Na1 O32 90.40(4) 2_756 1_655 ?
O120 Na1 O21 141.90(4) . . ?
O22 Na1 O21 88.69(4) 2_756 . ?
O32 Na1 O21 117.64(4) 1_655 . ?
O120 Na1 O110 84.48(4) . . ?
O22 Na1 O110 151.76(4) 2_756 . ?
O32 Na1 O110 81.78(4) 1_655 . ?
O21 Na1 O110 71.48(4) . . ?
O120 Na1 O130 84.51(4) . . ?
O22 Na1 O130 80.16(4) 2_756 . ?
O32 Na1 O130 160.61(5) 1_655 . ?
O21 Na1 O130 79.31(4) . . ?
O110 Na1 O130 114.22(4) . . ?
O120 Na1 Ni1 114.88(3) . . ?
O22 Na1 Ni1 121.97(3) 2_756 . ?
O32 Na1 Ni1 102.87(3) 1_655 . ?
O21 Na1 Ni1 35.21(2) . . ?
O110 Na1 Ni1 36.32(2) . . ?
O130 Na1 Ni1 96.48(3) . . ?
C2 O2 Ni1 105.49(7) . . ?
C2 O2 H2 102.2(14) . . ?
Ni1 O2 H2 105.5(14) . . ?
C10 O10 Ni1 126.13(9) . 2_766 ?
C21 O21 Ni1 112.32(8) . . ?
C21 O21 Na1 132.76(9) . . ?
Ni1 O21 Na1 102.24(4) . . ?
C21 O22 Na1 139.24(9) . 2_756 ?
C31 O31 Ni1 131.20(9) . . ?
C31 O32 Na1 138.65(9) . 1_455 ?
H100 O100 H101 103(2) . . ?
Ni1 O110 Na1 97.38(4) . . ?
Ni1 O110 H110 122.0(15) . . ?
Na1 O110 H110 122.8(15) . . ?
Ni1 O110 H111 103.9(14) . . ?
Na1 O110 H111 106.3(14) . . ?
H110 O110 H111 103(2) . . ?
Na1 O120 H120 131.2(16) . . ?
Na1 O120 H121 107.6(16) . . ?
H120 O120 H121 108(2) . . ?
Na1 O130 H130 93.5(18) . . ?
Na1 O130 H131 116.7(16) . . ?
H130 O130 H131 111(2) . . ?
Ni1 O140 H140 121.5(16) . . ?
Ni1 O140 H141 114.1(17) . . ?
H140 O140 H141 103(2) . . ?
C10 C1 C2 115.23(11) . . ?
C10 C1 H1A 108.5 . . ?
C2 C1 H1A 108.5 . . ?
C10 C1 H1B 108.5 . . ?
C2 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
O2 C2 C3 107.27(10) . . ?
O2 C2 C1 109.37(10) . . ?
C3 C2 C1 109.90(11) . . ?
O2 C2 C21 109.99(10) . . ?
C3 C2 C21 108.31(10) . . ?
C1 C2 C21 111.88(10) . . ?
C2 C3 C31 117.51(11) . . ?
C2 C3 H3A 107.9 . . ?
C31 C3 H3A 107.9 . . ?
C2 C3 H3B 107.9 . . ?
C31 C3 H3B 107.9 . . ?
H3A C3 H3B 107.2 . . ?
O11 C10 O10 123.86(12) . . ?
O11 C10 C1 118.39(12) . . ?
O10 C10 C1 117.71(11) . . ?
O22 C21 O21 125.38(13) . . ?
O22 C21 C2 117.64(12) . . ?
O21 C21 C2 116.88(11) . . ?
O32 C31 O31 123.00(12) . . ?
O32 C31 C3 116.84(12) . . ?
O31 C31 C3 120.16(11) . . ?
 
