data_General
_audit_creation_date                  '2006-06-09'
_audit_creation_method                'by CrystalStructure 3.7.0'
_audit_update_record                   ?

#==============================================================================

# PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic     ?
_journal_date_from_coeditor       ?
_journal_date_accepted            ?
_journal_coeditor_code            ?

#==============================================================================

# SUBMISSION DETAILS

_publ_contact_author_name             'Shin-ichiro Noro'
_publ_contact_author_address           
;                                       
    Research Institute for Electronic Science, Hokkaido University,
    N12W6, Kita-ku, Sapporo 060-0812, Japan
;                                       
_publ_contact_author_email            'noro@es.hokudai.ac.jp'
_publ_contact_author_fax              '+81-11-706-4972'
_publ_contact_author_phone            '+81-11-706-2884'
_publ_contact_letter
;
    ENTER TEXT OF LETTER
;
_publ_requested_journal               'ENTER JOURNAL NAME HERE'
_publ_requested_category              'CHOOSE FI FM FO CI CM CO or AD'
_publ_requested_coeditor_name          ?

#==============================================================================

# TITLE AND AUTHOR LIST

_publ_section_title
;
    ENTER SECTION TITLE
;
_publ_section_title_footnote
;
    ENTER FOOTNOTE TO TITLE OF PAPER
;
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
' FIRST AUTHORS NAME '
;
  FIRST AUTHORS FOOTNOTES
;
;
  FIRST AUTHORS ADDRESS
;
_publ_section_synopsis
;
  ENTER SYNOPSIS
;

#==============================================================================

# TEXT

_publ_section_abstract
;
    ENTER ABSTRACT
;
_publ_section_comment
;
    ENTER TEXT
;
_publ_section_references
;
    ENTER OTHER REFERENCES

    Rigaku/MSC and Rigaku Corporation. (2005).
    CrystalStructure 3.7.0.
    Single Crystal Structure Analysis Software.
    Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209.
    Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan.

    Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996)
    CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK.

;
_publ_section_figure_captions
;
    ENTER FIGURE CAPTIONS
;
_publ_section_exptl_prep
;
    ENTER COMPOUND PREPARATION DETAILS
;
_publ_section_exptl_refinement
;
    ENTER SPECIAL DETAILS OF THE REFINEMENT
;

#==============================================================================

data__060601test

#==============================================================================

# CHEMICAL DATA

_chemical_formula_sum                  'C18 H22 Ni3 O20 '
_chemical_formula_moiety               'C18 H22 Ni3 O20 '
_chemical_formula_weight               734.46
_chemical_melting_point                ?

#==============================================================================

# CRYSTAL DATA
_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_site_id
_symmetry_equiv_pos_as_xyz
1   '+X,+Y,+Z'
2   '-X,-Y,-Z'

#------------------------------------------------------------------------------

_cell_length_a                         6.6978(5)
_cell_length_b                         9.6542(8)
_cell_length_c                         10.1056(7)
_cell_angle_alpha                      112.708(3)
_cell_angle_beta                       93.919(2)
_cell_angle_gamma                      106.591(2)
_cell_volume                           565.79(7)
_cell_formula_units_Z                  1
_cell_measurement_reflns_used          4936
_cell_measurement_theta_min            3.2
_cell_measurement_theta_max            27.4
_cell_measurement_temperature          393.1

#------------------------------------------------------------------------------

_exptl_crystal_description            'block'
_exptl_crystal_colour                 'green'
_exptl_crystal_size_max                0.50
_exptl_crystal_size_mid                0.43
_exptl_crystal_size_min                0.33
_exptl_crystal_density_diffrn          2.155
_exptl_crystal_density_meas            ?
_exptl_crystal_density_method         'not measured'
_exptl_crystal_F_000                   374.00
_exptl_absorpt_coefficient_mu          2.577
_exptl_absorpt_correction_type         multi-scan
_exptl_absorpt_process_details         
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_absorpt_correction_T_min        0.378
_exptl_absorpt_correction_T_max        0.427

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_radiation_type                'Mo K\a'
_diffrn_radiation_wavelength           0.71075
_diffrn_measurement_device_type       'Rigaku RAXIS-RAPID'
_diffrn_measurement_method             ω
_diffrn_detector_area_resol_mean       10.00
_diffrn_reflns_number                  5537
_diffrn_reflns_av_R_equivalents        0.021
_diffrn_reflns_theta_max               27.46
_diffrn_measured_fraction_theta_max    0.989
_diffrn_reflns_theta_full              27.46
_diffrn_measured_fraction_theta_full   0.989
_diffrn_reflns_limit_h_min             -8
_diffrn_reflns_limit_h_max             8
_diffrn_reflns_limit_k_min             -12
_diffrn_reflns_limit_k_max             12
_diffrn_reflns_limit_l_min             -12
_diffrn_reflns_limit_l_max             13

#==============================================================================

# REFINEMENT DATA

_refine_special_details
;
    Refinement using reflections with F² > 2.0 sigma(F²).
    The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are 
    based on F, with F set to zero for negative F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_reflns_number_total                   2557
_reflns_number_gt                      2385
_reflns_threshold_expression           F²>2.0σ(F²)
_refine_ls_structure_factor_coef       Fsqd
_refine_ls_R_factor_gt                 0.0289
_refine_ls_wR_factor_ref               0.0836
_refine_ls_hydrogen_treatment          refall
_refine_ls_number_reflns               2557
_refine_ls_number_parameters           196
_refine_ls_goodness_of_fit_ref         1.166
_refine_ls_weighting_scheme            calc
_refine_ls_weighting_details
   'w = 1/[σ²(Fo²)+(0.0465P)²+0.3759P] where P=(Fo²+2Fc²)/3'
_refine_ls_shift/su_max                0.0010
_refine_diff_density_max               0.66
_refine_diff_density_min               -0.46
_refine_ls_extinction_method           none
_refine_ls_extinction_coef             ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
  'C' 'C'  0.003 0.002 
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
  'H' 'H'  0.000 0.000 
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
  'Ni' 'Ni'  0.339 1.112 
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
  'O' 'O'  0.011 0.006 
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================

# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
 Ni(1) Ni 0.0000 1.0000 0.5000 0.01543(11) Uani 1.00 2 d S . .
 Ni(2) Ni 0.08490(4) 0.63815(3) 0.26665(3) 0.01961(11) Uani 1.00 1 d . . .
 O(1) O 0.2145(2) 1.01666(19) 0.36835(16) 0.0251(3) Uani 1.00 1 d . . .
 O(2) O 0.1009(2) 0.78569(19) 0.16484(17) 0.0235(3) Uani 1.00 1 d . . .
 O(3) O 0.1344(3) 0.8138(2) -0.31328(18) 0.0313(3) Uani 1.00 1 d . . .
 O(4) O 0.2389(2) 1.05095(19) -0.32138(17) 0.0248(3) Uani 1.00 1 d . . .
 O(5) O 0.7774(2) 1.4825(2) 0.16063(17) 0.0293(3) Uani 1.00 1 d . . .
 O(6) O 0.5993(2) 1.5255(2) 0.34333(19) 0.0344(4) Uani 1.00 1 d . . .
 O(7) O -0.0422(2) 0.76073(18) 0.43492(16) 0.0198(3) Uani 1.00 1 d . . .
 O(8) O 0.1965(3) 0.5004(2) 0.09560(19) 0.0336(4) Uani 1.00 1 d . . .
 O(9) O 0.1204(3) 0.4889(2) 0.3644(2) 0.0426(4) Uani 1.00 1 d . . .
 O(10) O 0.3936(2) 0.7706(2) 0.3854(2) 0.0416(4) Uani 1.00 1 d . . .
 C(1) C 0.2627(3) 1.0276(2) 0.1435(2) 0.0167(3) Uani 1.00 1 d . . .
 C(2) C 0.2159(3) 0.9542(2) -0.0091(2) 0.0173(3) Uani 1.00 1 d . . .
 C(3) C 0.2845(3) 1.0424(2) -0.0887(2) 0.0166(3) Uani 1.00 1 d . . .
 C(4) C 0.4127(3) 1.2025(2) -0.0155(2) 0.0191(3) Uani 1.00 1 d . . .
 C(5) C 0.4670(3) 1.2749(2) 0.1367(2) 0.0185(3) Uani 1.00 1 d . . .
 C(6) C 0.3855(3) 1.1893(2) 0.2162(2) 0.0185(3) Uani 1.00 1 d . . .
 C(7) C 0.1861(3) 0.9360(2) 0.2322(2) 0.0179(3) Uani 1.00 1 d . . .
 C(8) C 0.2166(3) 0.9635(2) -0.2528(2) 0.0197(4) Uani 1.00 1 d . . .
 C(9) C 0.6233(3) 1.4407(2) 0.2201(2) 0.0211(4) Uani 1.00 1 d . . .
 H(1) H 0.1385 0.8458 -0.0580 0.021 Uiso 1.00 1 c R . .
 H(2) H 0.4618 1.2609 -0.0685 0.023 Uiso 1.00 1 c R . .
 H(3) H 0.4129 1.2400 0.3179 0.022 Uiso 1.00 1 c R . .
 H(4) H -0.179(6) 0.685(5) 0.403(4) 0.059(11) Uiso 1.00 1 c . . .
 H(5) H 0.039(6) 0.782(5) 0.534(4) 0.066(12) Uiso 1.00 1 c . . .



#==============================================================================

_computing_data_collection            'PROCESS-AUTO'
_computing_cell_refinement            'PROCESS-AUTO'
_computing_data_reduction             'CrystalStructure'
_computing_structure_solution         '?'
_computing_structure_refinement       'SHELXL'
_computing_publication_material       'CrystalStructure 3.7.0'
_computing_molecular_graphics          ?

#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details
;
    ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ni(1) O(1) 2.0380(17) ? . .
Ni(1) O(1) 2.0380(17) ? . 57602
Ni(1) O(4) 2.1284(17) ? . 55601
Ni(1) O(4) 2.1284(17) ? . 57502
Ni(1) O(7) 2.0681(17) ? . .
Ni(1) O(7) 2.0681(17) ? . 57602
Ni(2) O(2) 2.039(2) ? . .
Ni(2) O(5) 2.0823(14) ? . 44501
Ni(2) O(7) 2.0583(16) ? . .
Ni(2) O(8) 2.0698(19) ? . .
Ni(2) O(9) 2.091(2) ? . .
Ni(2) O(10) 2.0778(17) ? . .
O(1) C(7) 1.260(2) ? . .
O(2) C(7) 1.267(2) ? . .
O(3) C(8) 1.258(2) ? . .
O(4) C(8) 1.269(3) ? . .
O(5) C(9) 1.274(3) ? . .
O(6) C(9) 1.250(2) ? . .
C(1) C(2) 1.394(2) ? . .
C(1) C(6) 1.397(2) ? . .
C(1) C(7) 1.505(3) ? . .
C(2) C(3) 1.393(3) ? . .
C(3) C(4) 1.395(2) ? . .
C(3) C(8) 1.503(2) ? . .
C(4) C(5) 1.390(2) ? . .
C(5) C(6) 1.393(3) ? . .
C(5) C(9) 1.500(2) ? . .
O(7) H(4) 0.93(3) ? . .
O(7) H(5) 1.02(4) ? . .
C(2) H(1) 0.930 ? . .
C(4) H(2) 0.930 ? . .
C(6) H(3) 0.930 ? . .

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
O(1) Ni(1) O(1) 180.00(9) ? . . 57602
O(1) Ni(1) O(4) 92.52(6) ? . . 55601
O(1) Ni(1) O(4) 87.48(6) ? . . 57502
O(1) Ni(1) O(7) 90.67(6) ? . . .
O(1) Ni(1) O(7) 89.33(6) ? . . 57602
O(1) Ni(1) O(4) 87.48(6) ? 57602 . 55601
O(1) Ni(1) O(4) 92.52(6) ? 57602 . 57502
O(1) Ni(1) O(7) 89.33(6) ? 57602 . .
O(1) Ni(1) O(7) 90.67(6) ? 57602 . 57602
O(4) Ni(1) O(4) 180.00(9) ? 55601 . 57502
O(4) Ni(1) O(7) 87.91(6) ? 55601 . .
O(4) Ni(1) O(7) 92.09(6) ? 55601 . 57602
O(4) Ni(1) O(7) 92.09(6) ? 57502 . .
O(4) Ni(1) O(7) 87.91(6) ? 57502 . 57602
O(7) Ni(1) O(7) 0(440) ? . . 57602
O(2) Ni(2) O(5) 97.05(7) ? . . 44501
O(2) Ni(2) O(7) 95.23(7) ? . . .
O(2) Ni(2) O(8) 87.43(8) ? . . .
O(2) Ni(2) O(9) 170.25(8) ? . . .
O(2) Ni(2) O(10) 91.17(9) ? . . .
O(5) Ni(2) O(7) 88.17(6) ? 44501 . .
O(5) Ni(2) O(8) 88.55(6) ? 44501 . .
O(5) Ni(2) O(9) 89.91(8) ? 44501 . .
O(5) Ni(2) O(10) 171.73(10) ? 44501 . .
O(7) Ni(2) O(8) 176.01(6) ? . . .
O(7) Ni(2) O(9) 91.79(8) ? . . .
O(7) Ni(2) O(10) 92.04(7) ? . . .
O(8) Ni(2) O(9) 85.92(9) ? . . .
O(8) Ni(2) O(10) 90.88(7) ? . . .
O(9) Ni(2) O(10) 81.82(9) ? . . .
Ni(1) O(1) C(7) 127.51(13) ? . . .
Ni(2) O(2) C(7) 122.49(15) ? . . .
Ni(1) O(4) C(8) 121.32(11) ? 55401 . .
Ni(2) O(5) C(9) 127.07(13) ? 66501 . .
Ni(1) O(7) Ni(2) 122.16(8) ? . . .
C(2) C(1) C(6) 119.4(2) ? . . .
C(2) C(1) C(7) 121.44(16) ? . . .
C(6) C(1) C(7) 119.12(18) ? . . .
C(1) C(2) C(3) 120.37(17) ? . . .
C(2) C(3) C(4) 119.73(18) ? . . .
C(2) C(3) C(8) 119.25(16) ? . . .
C(4) C(3) C(8) 121.0(2) ? . . .
C(3) C(4) C(5) 120.1(2) ? . . .
C(4) C(5) C(6) 119.86(17) ? . . .
C(4) C(5) C(9) 122.2(2) ? . . .
C(6) C(5) C(9) 117.80(18) ? . . .
C(1) C(6) C(5) 120.22(18) ? . . .
O(1) C(7) O(2) 125.7(2) ? . . .
O(1) C(7) C(1) 116.47(18) ? . . .
O(2) C(7) C(1) 117.83(17) ? . . .
O(3) C(8) O(4) 123.94(19) ? . . .
O(3) C(8) C(3) 117.4(2) ? . . .
O(4) C(8) C(3) 118.59(18) ? . . .
O(5) C(9) O(6) 124.66(17) ? . . .
O(5) C(9) C(5) 116.43(17) ? . . .
O(6) C(9) C(5) 118.9(2) ? . . .
Ni(1) O(7) H(4) 120(3) ? . . .
Ni(1) O(7) H(5) 92(2) ? . . .
Ni(2) O(7) H(4) 96(2) ? . . .
Ni(2) O(7) H(5) 111(2) ? . . .
H(4) O(7) H(5) 117(4) ? . . .
C(1) C(2) H(1) 119.8 ? . . .
C(3) C(2) H(1) 119.8 ? . . .
C(3) C(4) H(2) 119.9 ? . . .
C(5) C(4) H(2) 119.9 ? . . .
C(1) C(6) H(3) 119.9 ? . . .
C(5) C(6) H(3) 119.9 ? . . .

#==============================================================================

#     End of CIF

#==============================================================================

