#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:39:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179255 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/75/4317565.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_4317565
loop_
_publ_author_name
'Chih-Chieh Wang'
'Cheng-Han Yang'
'Gene-Hsiang Lee'
_publ_section_title
;
 Synthesis and Structural Characterization of [Na2M(C5O5)2(H2O)2].4H2O (M
 = NiII, CuII)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1015
_journal_page_last               1018
_journal_paper_doi               10.1021/ic0108538
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C10 H12 Na2 Ni O16'
_chemical_formula_weight         492.89
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                100.54(2)
_cell_angle_beta                 111.74(2)
_cell_angle_gamma                99.622(15)
_cell_formula_units_Z            1
_cell_length_a                   6.9223(14)
_cell_length_b                   7.9382(13)
_cell_length_c                   8.703(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      16.38
_cell_measurement_theta_min      7.36
_cell_volume                     422.03(17)
_computing_cell_refinement       'Nonius CAD4'
_computing_data_collection       'Nonius CAD4'
_computing_data_reduction        'NRCSDP DATRD2'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       'ω--2θ scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2454
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.290
_exptl_absorpt_correction_T_max  0.7882
_exptl_absorpt_correction_T_min  0.6913
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             250
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.073
_refine_ls_goodness_of_fit_obs   1.110
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_obs          0.0250
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0401P)²+0.0795P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0703
_refine_ls_wR_factor_obs         0.0683
_reflns_number_observed          2182
_reflns_number_total             2454
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0108538_1.cif
_cod_data_source_block           ic7528
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.0795P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.0795P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        422.00(14)
_cod_database_code               4317565
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni1 Ni 0.5000 0.5000 0.5000 0.02000(8) Uani 1 d S .
Na1 Na 0.74290(10) 0.50463(8) 0.99312(8) 0.03083(14) Uani 1 d . .
O1 O 0.6147(2) 0.66085(12) 0.75486(12) 0.0253(2) Uani 1 d . .
O2 O 0.6181(2) 0.73243(12) 0.45534(12) 0.0253(2) Uani 1 d . .
O3 O 0.8069(2) 1.11455(14) 0.51951(15) 0.0350(3) Uani 1 d . .
O4 O 1.0998(2) 0.71685(13) 1.11959(14) 0.0288(2) Uani 1 d . .
O5 O 0.7604(2) 1.00484(13) 1.02614(13) 0.0300(2) Uani 1 d . .
O6 O 0.7882(2) 0.44736(15) 0.5423(2) 0.0293(2) Uani 1 d . .
H6A H 0.8006(36) 0.3494(33) 0.5540(29) 0.046(6) Uiso 1 d . .
H6B H 0.8869(46) 0.5230(38) 0.6222(35) 0.065(8) Uiso 1 d . .
O7 O 0.8305(2) 0.3517(2) 1.2130(2) 0.0338(3) Uani 1 d . .
H7A H 0.7641(41) 0.3528(34) 1.2691(33) 0.055(7) Uiso 1 d . .
H7B H 0.8104(39) 0.2571(32) 1.1706(31) 0.048(7) Uiso 1 d . .
O8 O 0.6053(2) 0.7068(2) 1.13087(15) 0.0308(2) Uani 1 d . .
H8A H 0.6428(41) 0.7312(33) 1.2265(35) 0.056(7) Uiso 1 d . .
H8B H 0.6417(38) 0.7955(34) 1.1112(32) 0.052(7) Uiso 1 d . .
C1 C 0.6817(2) 0.8163(2) 0.7477(2) 0.0199(2) Uani 1 d . .
C2 C 0.6884(2) 0.8522(2) 0.5938(2) 0.0199(2) Uani 1 d . .
C3 C 0.7786(2) 1.0400(2) 0.6242(2) 0.0217(2) Uani 1 d . .
C4 C 0.8229(2) 1.1238(2) 0.8055(2) 0.0208(2) Uani 1 d . .
C5 C 0.7549(2) 0.9829(2) 0.8796(2) 0.0207(2) Uani 1 d . .
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'
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
_geom_angle_publ_flag
O6 Ni1 O6 180.0 . 2_666 ?
O6 Ni1 O2 92.50(5) . 2_666 ?
O6 Ni1 O2 87.50(5) 2_666 2_666 ?
O6 Ni1 O2 87.50(5) . . ?
O6 Ni1 O2 92.50(5) 2_666 . ?
O2 Ni1 O2 180.0 2_666 . ?
O6 Ni1 O1 92.23(5) . . ?
O6 Ni1 O1 87.77(5) 2_666 . ?
O2 Ni1 O1 96.70(4) 2_666 . ?
O2 Ni1 O1 83.30(4) . . ?
O6 Ni1 O1 87.77(5) . 2_666 ?
O6 Ni1 O1 92.23(5) 2_666 2_666 ?
O2 Ni1 O1 83.30(4) 2_666 2_666 ?
O2 Ni1 O1 96.70(4) . 2_666 ?
O1 Ni1 O1 180.0 . 2_666 ?
O8 Na1 O7 94.85(5) . . ?
O8 Na1 O8 89.37(5) . 2_667 ?
O7 Na1 O8 85.14(5) . 2_667 ?
O8 Na1 O4 173.38(5) . 2_767 ?
O7 Na1 O4 78.60(5) . 2_767 ?
O8 Na1 O4 91.04(5) 2_667 2_767 ?
O8 Na1 O4 91.23(5) . . ?
O7 Na1 O4 94.41(5) . . ?
O8 Na1 O4 179.27(5) 2_667 . ?
O4 Na1 O4 88.31(4) 2_767 . ?
O8 Na1 O1 82.55(4) . . ?
O7 Na1 O1 174.95(5) . . ?
O8 Na1 O1 90.49(5) 2_667 . ?
O4 Na1 O1 104.05(4) 2_767 . ?
O4 Na1 O1 89.99(5) . . ?
O8 Na1 Na1 45.38(4) . 2_667 ?
O7 Na1 Na1 89.91(4) . 2_667 ?
O8 Na1 Na1 44.00(3) 2_667 2_667 ?
O4 Na1 Na1 134.66(4) 2_767 2_667 ?
O4 Na1 Na1 136.61(4) . 2_667 ?
O1 Na1 Na1 85.18(4) . 2_667 ?
O8 Na1 Na1 134.95(5) . 2_767 ?
O7 Na1 Na1 85.18(4) . 2_767 ?
O8 Na1 Na1 135.26(4) 2_667 2_767 ?
O4 Na1 Na1 44.22(3) 2_767 2_767 ?
O4 Na1 Na1 44.09(3) . 2_767 ?
O1 Na1 Na1 99.72(4) . 2_767 ?
Na1 Na1 Na1 175.10(4) 2_667 2_767 ?
C1 O1 Ni1 105.00(8) . . ?
C1 O1 Na1 131.61(9) . . ?
Ni1 O1 Na1 115.90(4) . . ?
C2 O2 Ni1 107.31(8) . . ?
C4 O4 Na1 130.86(10) 2_777 2_767 ?
C4 O4 Na1 137.07(10) 2_777 . ?
Na1 O4 Na1 91.69(4) 2_767 . ?
Na1 O8 Na1 90.63(5) . 2_667 ?
O1 C1 C2 121.98(11) . . ?
O1 C1 C5 129.09(12) . . ?
C2 C1 C5 108.91(11) . . ?
O2 C2 C1 122.13(11) . . ?
O2 C2 C3 127.76(12) . . ?
C1 C2 C3 110.09(11) . . ?
O3 C3 C2 126.68(12) . . ?
O3 C3 C4 127.23(12) . . ?
C2 C3 C4 106.06(11) . . ?
O4 C4 C5 126.01(12) 2_777 . ?
O4 C4 C3 125.94(12) 2_777 . ?
C5 C4 C3 108.04(11) . . ?
O5 C5 C1 127.18(12) . . ?
O5 C5 C4 126.08(12) . . ?
C1 C5 C4 106.75(11) . . ?
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 O6 2.0199(12) . ?
Ni1 O6 2.0199(12) 2_666 ?
Ni1 O2 2.0536(10) 2_666 ?
Ni1 O2 2.0537(10) . ?
Ni1 O1 2.1213(11) . ?
Ni1 O1 2.1213(11) 2_666 ?
Na1 O8 2.3606(14) . ?
Na1 O7 2.396(2) . ?
Na1 O8 2.419(2) 2_667 ?
Na1 O4 2.4577(13) 2_767 ?
Na1 O4 2.4633(14) . ?
Na1 O1 2.5632(13) . ?
Na1 Na1 3.3982(14) 2_667 ?
Na1 Na1 3.5305(14) 2_767 ?
O1 C1 1.265(2) . ?
O2 C2 1.259(2) . ?
O3 C3 1.229(2) . ?
O4 C4 1.235(2) 2_777 ?
O4 Na1 2.4577(13) 2_767 ?
O5 C5 1.241(2) . ?
O8 Na1 2.419(2) 2_667 ?
C1 C2 1.435(2) . ?
C1 C5 1.453(2) . ?
C2 C3 1.451(2) . ?
C3 C4 1.488(2) . ?
C4 O4 1.235(2) 2_777 ?
C4 C5 1.484(2) . ?
