# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Ryo Sekiya'
_publ_contact_author_email       CSEKIYA@MAIL.ECC.U-TOKYO.AC.JP

_publ_section_title              
;
Synergistic interplay of metal-ligand coordination
and hydrogen bond interaction: a facile route for the construction
of MOFs with inclusion ability to relatively large aromatic molecules
;
loop_
_publ_author_name
'Ryo Sekiya'
'Reiko Kuroda'
'Shinichi Nishikiori'

data_pyrene_inclusion_compound1
_database_code_depnum_ccdc_archive 'CCDC 727046'

_audit_creation_date             2009-01-09T17:52:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C14 H12 N6 Ni O2 S2, C8 H5'
_chemical_formula_sum            'C22 H17 N6 Ni O2 S2'
_chemical_formula_weight         520.25

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   C2/c
_symmetry_Int_Tables_number      15

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   32.418(3)
_cell_length_b                   9.5238(8)
_cell_length_c                   15.9371(16)
_cell_angle_alpha                90
_cell_angle_beta                 118.442(5)
_cell_angle_gamma                90
_cell_volume                     4326.6(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    153(2)
_cell_measurement_theta_min      1.43
_cell_measurement_theta_max      29.95

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            'bluish green'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2136
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995'
_exptl_absorpt_correction_T_min  0.8959
_exptl_absorpt_correction_T_max  0.8959

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_probe          X-ray
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'RIGAKU RAXIS-RAPID'
_diffrn_measurement_method       ω
_diffrn_reflns_av_R_equivalents  0.152
_diffrn_reflns_av_unetI/netI     0.2387
_diffrn_reflns_number            24805
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         29.95
_diffrn_reflns_theta_full        29.95
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             6259
_reflns_number_gt                2759
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       RAPID-AUTO
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        RAPID-AUTO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
# 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)+(0.0515P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6259
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1617
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.14
_refine_ls_wR_factor_gt          0.0997
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_restrained_S_all      0.846
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.182

#----------------------------------------------------------------------------#
# 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
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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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_
_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
C1 C 0.77800(15) 0.8629(5) 0.5808(3) 0.0205(10) Uani 1 1 d . . .
C2 C 0.72186(15) 0.2695(5) 0.6711(3) 0.0187(10) Uani 1 1 d . . .
C11 C 0.82035(18) 0.3782(5) 0.6136(4) 0.0282(11) Uani 1 1 d . . .
H11 H 0.7951 0.3145 0.5969 0.034 Uiso 1 1 calc R . .
C12 C 0.85828(17) 0.3353(6) 0.6030(4) 0.0321(12) Uani 1 1 d . . .
H12 H 0.8593 0.2433 0.5809 0.038 Uiso 1 1 calc R . .
C13 C 0.89479(16) 0.4281(7) 0.6249(3) 0.0292(12) Uani 1 1 d . . .
C14 C 0.89209(16) 0.5590(6) 0.6575(3) 0.0308(12) Uani 1 1 d . . .
H14 H 0.9163 0.6259 0.6715 0.037 Uiso 1 1 calc R . .
C15 C 0.85378(15) 0.5929(6) 0.6698(3) 0.0274(11) Uani 1 1 d . . .
H15 H 0.8531 0.682 0.6959 0.033 Uiso 1 1 calc R . .
C16 C 0.93779(17) 0.3900(7) 0.6148(4) 0.0360(14) Uani 1 1 d . . .
C21 C 0.67926(16) 0.5932(5) 0.7049(3) 0.0227(10) Uani 1 1 d . . .
H21 H 0.6971 0.5211 0.7482 0.027 Uiso 1 1 calc R . .
C22 C 0.63780(16) 0.6368(5) 0.7024(3) 0.0238(11) Uani 1 1 d . . .
H22 H 0.6268 0.5918 0.7412 0.029 Uiso 1 1 calc R . .
C23 C 0.61283(16) 0.7452(6) 0.6434(3) 0.0254(11) Uani 1 1 d . . .
C24 C 0.62936(16) 0.8072(6) 0.5869(3) 0.0265(11) Uani 1 1 d . . .
H24 H 0.6129 0.8827 0.5454 0.032 Uiso 1 1 calc R . .
C25 C 0.67076(16) 0.7561(5) 0.5923(3) 0.0239(11) Uani 1 1 d . . .
H25 H 0.6824 0.7996 0.5541 0.029 Uiso 1 1 calc R . .
C26 C 0.56647(17) 0.7863(6) 0.6387(3) 0.0307(12) Uani 1 1 d . . .
N1 N 0.73875(13) 0.3747(4) 0.6675(2) 0.0204(8) Uani 1 1 d . . .
N2 N 0.76877(13) 0.7706(4) 0.6153(2) 0.0196(8) Uani 1 1 d . . .
N11 N 0.81752(13) 0.5049(4) 0.6464(2) 0.0215(9) Uani 1 1 d . . .
N12 N 0.95670(18) 0.2704(6) 0.6504(4) 0.0583(17) Uani 1 1 d . . .
H12A H 0.9819 0.2426 0.6475 0.07 Uiso 1 1 calc R . .
H12B H 0.9444 0.2165 0.6776 0.07 Uiso 1 1 calc R . .
N21 N 0.69490(13) 0.6497(4) 0.6480(3) 0.0199(9) Uani 1 1 d . . .
N22 N 0.54495(15) 0.8971(5) 0.5892(3) 0.0414(13) Uani 1 1 d . . .
H22A H 0.5186 0.9253 0.5871 0.05 Uiso 1 1 calc R . .
H22B H 0.5567 0.9437 0.5578 0.05 Uiso 1 1 calc R . .
O11 O 0.95261(13) 0.4714(5) 0.5757(3) 0.0485(12) Uani 1 1 d . . .
O21 O 0.55184(12) 0.7166(5) 0.6841(3) 0.0424(11) Uani 1 1 d . . .
S1 S 0.79120(4) 0.99180(14) 0.52844(8) 0.0240(3) Uani 1 1 d . . .
S2 S 0.69778(4) 0.11928(14) 0.67588(8) 0.0231(3) Uani 1 1 d . . .
Ni1 Ni 0.75576(2) 0.57431(7) 0.64825(4) 0.01655(14) Uani 1 1 d . . .
C101 C 0.4619(2) 0.6913(9) 0.3764(5) 0.066(2) Uani 1 1 d . . .
H101 H 0.4545 0.7625 0.3296 0.079 Uiso 1 1 calc R . .
C102 C 0.5056(2) 0.6197(8) 0.4104(4) 0.0515(18) Uani 1 1 d . . .
C103 C 0.5366(3) 0.6453(10) 0.3793(5) 0.077(3) Uani 1 1 d . . .
H103 H 0.5294 0.7145 0.3313 0.092 Uiso 1 1 calc R . .
C104 C 0.51631(19) 0.5145(8) 0.4823(4) 0.0450(16) Uani 1 1 d . . .
C105 C 0.5591(2) 0.4407(8) 0.5205(5) 0.0525(18) Uani 1 1 d . . .
C106 C 0.5907(2) 0.4743(9) 0.4853(5) 0.067(2) Uani 1 1 d . . .
H106 H 0.6201 0.428 0.51 0.08 Uiso 1 1 calc R . .
C107 C 0.4318(3) 0.6646(9) 0.4058(5) 0.073(2) Uani 1 1 d . . .
H107 H 0.403 0.7148 0.3789 0.087 Uiso 1 1 calc R . .
C108 C 0.5782(3) 0.5758(11) 0.4139(5) 0.085(3) Uani 1 1 d . . .
H108 H 0.599 0.5966 0.3893 0.103 Uiso 1 1 calc R . .


#----------------------------------------------------------------------------#
# 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
C1 N2 1.149(6) . ?
C1 S1 1.651(5) . ?
C2 N1 1.156(6) . ?
C2 S2 1.649(5) . ?
C11 N11 1.335(6) . ?
C11 C12 1.381(6) . ?
C11 H11 0.95 . ?
C12 C13 1.382(7) . ?
C12 H12 0.95 . ?
C13 C14 1.369(8) . ?
C13 C16 1.521(6) . ?
C14 C15 1.385(6) . ?
C14 H14 0.95 . ?
C15 N11 1.344(6) . ?
C15 H15 0.95 . ?
C16 O11 1.226(6) . ?
C16 N12 1.290(7) . ?
C21 N21 1.345(5) . ?
C21 C22 1.389(6) . ?
C21 H21 0.95 . ?
C22 C23 1.371(7) . ?
C22 H22 0.95 . ?
C23 C24 1.381(6) . ?
C23 C26 1.519(6) . ?
C24 C25 1.391(6) . ?
C24 H24 0.95 . ?
C25 N21 1.329(6) . ?
C25 H25 0.95 . ?
C26 O21 1.232(6) . ?
C26 N22 1.302(7) . ?
N1 Ni1 2.043(4) . ?
N2 Ni1 2.040(4) . ?
N11 Ni1 2.122(4) . ?
N12 H12A 0.88 . ?
N12 H12B 0.88 . ?
N21 Ni1 2.098(4) . ?
N22 H22A 0.88 . ?
N22 H22B 0.88 . ?
S1 Ni1 2.5612(13) 7_666 ?
S2 Ni1 2.5074(13) 4_646 ?
Ni1 S2 2.5074(13) 4_656 ?
Ni1 S1 2.5612(13) 7_666 ?
C101 C107 1.292(9) . ?
C101 C102 1.425(10) . ?
C101 H101 0.95 . ?
C102 C103 1.340(8) . ?
C102 C104 1.435(9) . ?
C103 C108 1.360(11) . ?
C103 H103 0.95 . ?
C104 C105 1.409(8) . ?
C104 C104 1.442(11) 5_666 ?
C105 C106 1.419(9) . ?
C105 C107 1.463(10) 5_666 ?
C106 C108 1.398(11) . ?
C106 H106 0.95 . ?
C107 C105 1.463(10) 5_666 ?
C107 H107 0.95 . ?
C108 H108 0.95 . ?

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
N2 C1 S1 178.1(4) . . ?
N1 C2 S2 179.8(4) . . ?
N11 C11 C12 123.1(5) . . ?
N11 C11 H11 118.4 . . ?
C12 C11 H11 118.4 . . ?
C11 C12 C13 119.0(5) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
C14 C13 C12 118.5(4) . . ?
C14 C13 C16 119.0(5) . . ?
C12 C13 C16 122.6(5) . . ?
C13 C14 C15 119.3(5) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
N11 C15 C14 122.7(5) . . ?
N11 C15 H15 118.7 . . ?
C14 C15 H15 118.7 . . ?
O11 C16 N12 124.2(5) . . ?
O11 C16 C13 120.2(5) . . ?
N12 C16 C13 115.6(5) . . ?
N21 C21 C22 122.1(4) . . ?
N21 C21 H21 119 . . ?
C22 C21 H21 119 . . ?
C23 C22 C21 119.5(4) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 118.9(4) . . ?
C22 C23 C26 118.4(4) . . ?
C24 C23 C26 122.6(5) . . ?
C23 C24 C25 118.2(5) . . ?
C23 C24 H24 120.9 . . ?
C25 C24 H24 120.9 . . ?
N21 C25 C24 123.4(4) . . ?
N21 C25 H25 118.3 . . ?
C24 C25 H25 118.3 . . ?
O21 C26 N22 123.2(4) . . ?
O21 C26 C23 118.7(5) . . ?
N22 C26 C23 118.1(4) . . ?
C2 N1 Ni1 169.1(4) . . ?
C1 N2 Ni1 163.1(3) . . ?
C11 N11 C15 117.3(4) . . ?
C11 N11 Ni1 121.9(3) . . ?
C15 N11 Ni1 120.5(3) . . ?
C16 N12 H12A 120 . . ?
C16 N12 H12B 120 . . ?
H12A N12 H12B 120 . . ?
C25 N21 C21 117.7(4) . . ?
C25 N21 Ni1 121.1(3) . . ?
C21 N21 Ni1 121.2(3) . . ?
C26 N22 H22A 120 . . ?
C26 N22 H22B 120 . . ?
H22A N22 H22B 120 . . ?
C1 S1 Ni1 102.19(16) . 7_666 ?
C2 S2 Ni1 98.88(16) . 4_646 ?
N2 Ni1 N1 174.47(14) . . ?
N2 Ni1 N21 89.73(15) . . ?
N1 Ni1 N21 89.90(15) . . ?
N2 Ni1 N11 88.28(15) . . ?
N1 Ni1 N11 92.05(15) . . ?
N21 Ni1 N11 177.98(16) . . ?
N2 Ni1 S2 92.50(10) . 4_656 ?
N1 Ni1 S2 93.02(11) . 4_656 ?
N21 Ni1 S2 90.41(10) . 4_656 ?
N11 Ni1 S2 90.02(10) . 4_656 ?
N2 Ni1 S1 91.71(10) . 7_666 ?
N1 Ni1 S1 82.78(11) . 7_666 ?
N21 Ni1 S1 90.93(11) . 7_666 ?
N11 Ni1 S1 88.79(10) . 7_666 ?
S2 Ni1 S1 175.60(5) 4_656 7_666 ?
C107 C101 C102 123.5(7) . . ?
C107 C101 H101 118.3 . . ?
C102 C101 H101 118.3 . . ?
C103 C102 C101 123.9(7) . . ?
C103 C102 C104 118.9(7) . . ?
C101 C102 C104 117.2(6) . . ?
C102 C103 C108 122.4(8) . . ?
C102 C103 H103 118.8 . . ?
C108 C103 H103 118.8 . . ?
C105 C104 C102 120.5(6) . . ?
C105 C104 C104 119.3(8) . 5_666 ?
C102 C104 C104 120.1(7) . 5_666 ?
C104 C105 C106 117.7(7) . . ?
C104 C105 C107 117.9(6) . 5_666 ?
C106 C105 C107 124.4(7) . 5_666 ?
C108 C106 C105 119.6(7) . . ?
C108 C106 H106 120.2 . . ?
C105 C106 H106 120.2 . . ?
C101 C107 C105 121.9(7) . 5_666 ?
C101 C107 H107 119.1 . . ?
C105 C107 H107 119.1 5_666 . ?
C103 C108 C106 120.9(7) . . ?
C103 C108 H108 119.6 . . ?
C106 C108 H108 119.6 . . ?

#===END

data_anthraquinone_inclusion_compound2
_database_code_depnum_ccdc_archive 'CCDC 727047'

_audit_creation_date             2009-01-10T11:48:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C14 H12 N6 Ni O2 S2, C7 H4 O1'
_chemical_formula_sum            'C21 H16 N6 Ni O3 S2'
_chemical_formula_weight         523.22

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9523(6)
_cell_length_b                   10.9632(6)
_cell_length_c                   16.9567(10)
_cell_angle_alpha                90.564(4)
_cell_angle_beta                 65.422(3)
_cell_angle_gamma                56.997(9)
_cell_volume                     1071.93(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_theta_min      1.39
_cell_measurement_theta_max      29.98

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             536
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995'
_exptl_absorpt_correction_T_min  0.8478
_exptl_absorpt_correction_T_max  0.8947

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_probe          X-ray
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'RIGAKU RAXIS-RAPID'
_diffrn_measurement_method       ω
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_number            11387
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.39
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_full        29.98
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_reflns_number_total             5927
_reflns_number_gt                4173
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       RAPID-AUTO
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        RAPID-AUTO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
# 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)+(0.0781P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5927
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.043
_refine_ls_wR_factor_ref         0.1336
_refine_ls_wR_factor_gt          0.1096
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.141

#----------------------------------------------------------------------------#
# 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
C C 0.003 0.002 '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'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.125 0.123 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.339 1.112 '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
C1 C -0.2722(5) 0.5973(3) 0.05915(18) 0.0165(5) Uani 1 1 d . . .
C2 C 0.2788(5) -0.1131(3) -0.05297(18) 0.0162(5) Uani 1 1 d . . .
C11 C -0.1216(5) 0.3379(3) -0.1316(2) 0.0200(6) Uani 1 1 d . . .
H11 H -0.2562 0.422 -0.0792 0.024 Uiso 1 1 calc R . .
C12 C -0.1081(5) 0.3407(3) -0.2152(2) 0.0206(6) Uani 1 1 d . . .
H12 H -0.2284 0.4273 -0.2201 0.025 Uiso 1 1 calc R . .
C13 C 0.0825(5) 0.2161(3) -0.2923(2) 0.0200(6) Uani 1 1 d . . .
C14 C 0.2525(6) 0.0931(3) -0.2812(2) 0.0246(6) Uani 1 1 d . . .
H14 H 0.382 0.0037 -0.3315 0.03 Uiso 1 1 calc R . .
C15 C 0.2313(5) 0.1021(3) -0.1960(2) 0.0231(6) Uani 1 1 d . . .
H15 H 0.3534 0.0193 -0.1899 0.028 Uiso 1 1 calc R . .
C16 C 0.0972(5) 0.2232(4) -0.3831(2) 0.0224(6) Uani 1 1 d . . .
C21 C 0.0643(5) 0.1344(3) 0.1695(2) 0.0200(6) Uani 1 1 d . . .
H21 H 0.0509 0.0631 0.1459 0.024 Uiso 1 1 calc R . .
C22 C 0.0867(5) 0.1280(3) 0.24644(19) 0.0207(6) Uani 1 1 d . . .
H22 H 0.0923 0.0519 0.274 0.025 Uiso 1 1 calc R . .
C23 C 0.1009(5) 0.2339(3) 0.28283(19) 0.0197(6) Uani 1 1 d . . .
C24 C 0.0967(5) 0.3416(3) 0.2388(2) 0.0204(6) Uani 1 1 d . . .
H24 H 0.1065 0.4157 0.2616 0.024 Uiso 1 1 calc R . .
C25 C 0.0780(5) 0.3384(3) 0.1610(2) 0.0210(6) Uani 1 1 d . . .
H25 H 0.0774 0.4109 0.1307 0.025 Uiso 1 1 calc R . .
C26 C 0.1179(5) 0.2286(4) 0.3681(2) 0.0230(6) Uani 1 1 d . . .
N1 N -0.1742(4) 0.4669(3) 0.04623(16) 0.0181(5) Uani 1 1 d . . .
N2 N 0.2277(4) 0.0073(3) -0.02886(17) 0.0195(5) Uani 1 1 d . . .
N11 N 0.0465(4) 0.2219(3) -0.12106(16) 0.0188(5) Uani 1 1 d . . .
N12 N 0.1799(5) 0.0946(3) -0.43977(19) 0.0330(7) Uani 1 1 d . . .
H12A H 0.1922 0.0929 -0.4939 0.04 Uiso 1 1 calc R . .
H12B H 0.2223 0.0115 -0.4231 0.04 Uiso 1 1 calc R . .
N21 N 0.0608(4) 0.2380(3) 0.12687(16) 0.0178(5) Uani 1 1 d . . .
N22 N 0.0801(5) 0.3485(3) 0.41316(19) 0.0308(6) Uani 1 1 d . . .
H22A H 0.087 0.3491 0.4636 0.037 Uiso 1 1 calc R . .
H22B H 0.0481 0.4273 0.3926 0.037 Uiso 1 1 calc R . .
O11 O 0.0349(4) 0.3433(3) -0.40224(15) 0.0273(5) Uani 1 1 d . . .
O21 O 0.1636(5) 0.1144(3) 0.39386(16) 0.0325(6) Uani 1 1 d . . .
S1 S -0.40565(13) 0.78163(8) 0.07507(5) 0.02053(16) Uani 1 1 d . . .
S2 S 0.34549(13) -0.28164(8) -0.08780(5) 0.02145(16) Uani 1 1 d . . .
Ni1 Ni 0.03932(6) 0.23623(4) 0.00642(2) 0.01521(11) Uani 1 1 d . . .
C101 C 0.5155(6) 0.5639(4) 0.2817(2) 0.0300(7) Uani 1 1 d . . .
H101 H 0.5299 0.5473 0.2234 0.036 Uiso 1 1 calc R . .
C102 C 0.5254(6) 0.4589(4) 0.3284(2) 0.0274(7) Uani 1 1 d . . .
H102 H 0.5421 0.3728 0.303 0.033 Uiso 1 1 calc R . .
C103 C 0.5106(5) 0.4809(4) 0.4125(2) 0.0222(6) Uani 1 1 d . . .
C104 C 0.5363(5) 0.3629(4) 0.4597(2) 0.0241(6) Uani 1 1 d . . .
C105 C 0.5192(5) 0.3901(4) 0.5498(2) 0.0232(6) Uani 1 1 d . . .
C106 C 0.5323(6) 0.2851(4) 0.5970(2) 0.0290(7) Uani 1 1 d . . .
H106 H 0.5532 0.1973 0.5711 0.035 Uiso 1 1 calc R . .
C107 C 0.5150(6) 0.3073(4) 0.6812(2) 0.0336(8) Uani 1 1 d . . .
H107 H 0.5239 0.2354 0.7133 0.04 Uiso 1 1 calc R . .
O101 O 0.5760(5) 0.2449(3) 0.42421(16) 0.0342(6) Uani 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
C1 N1 1.156(4) . ?
C1 S1 1.642(3) . ?
C2 N2 1.157(3) . ?
C2 S2 1.642(3) . ?
C11 N11 1.337(4) . ?
C11 C12 1.378(4) . ?
C11 H11 0.95 . ?
C12 C13 1.390(4) . ?
C12 H12 0.95 . ?
C13 C14 1.383(4) . ?
C13 C16 1.502(4) . ?
C14 C15 1.378(4) . ?
C14 H14 0.95 . ?
C15 N11 1.346(4) . ?
C15 H15 0.95 . ?
C16 O11 1.232(4) . ?
C16 N12 1.334(4) . ?
C21 N21 1.345(4) . ?
C21 C22 1.386(4) . ?
C21 H21 0.95 . ?
C22 C23 1.388(4) . ?
C22 H22 0.95 . ?
C23 C24 1.396(4) . ?
C23 C26 1.507(4) . ?
C24 C25 1.390(4) . ?
C24 H24 0.95 . ?
C25 N21 1.335(4) . ?
C25 H25 0.95 . ?
C26 O21 1.240(4) . ?
C26 N22 1.326(4) . ?
N1 Ni1 2.018(2) . ?
N2 Ni1 2.008(2) . ?
N11 Ni1 2.141(2) . ?
N12 H12A 0.88 . ?
N12 H12B 0.88 . ?
N21 Ni1 2.120(2) . ?
N22 H22A 0.88 . ?
N22 H22B 0.88 . ?
S1 Ni1 2.5414(9) 2_565 ?
S2 Ni1 2.5160(9) 2 ?
Ni1 S2 2.5160(9) 2 ?
Ni1 S1 2.5414(9) 2_565 ?
C101 C102 1.389(5) . ?
C101 C107 1.390(5) 2_666 ?
C101 H101 0.95 . ?
C102 C103 1.390(4) . ?
C102 H102 0.95 . ?
C103 C105 1.398(4) 2_666 ?
C103 C104 1.491(4) . ?
C104 O101 1.231(4) . ?
C104 C105 1.489(4) . ?
C105 C106 1.391(4) . ?
C105 C103 1.398(4) 2_666 ?
C106 C107 1.383(5) . ?
C106 H106 0.95 . ?
C107 C101 1.390(5) 2_666 ?
C107 H107 0.95 . ?

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
N1 C1 S1 178.5(3) . . ?
N2 C2 S2 178.4(3) . . ?
N11 C11 C12 122.8(3) . . ?
N11 C11 H11 118.6 . . ?
C12 C11 H11 118.6 . . ?
C11 C12 C13 119.6(3) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C14 C13 C12 117.8(3) . . ?
C14 C13 C16 123.4(3) . . ?
C12 C13 C16 118.8(3) . . ?
C15 C14 C13 119.0(3) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
N11 C15 C14 123.4(3) . . ?
N11 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
O11 C16 N12 123.3(3) . . ?
O11 C16 C13 120.1(3) . . ?
N12 C16 C13 116.6(3) . . ?
N21 C21 C22 122.4(3) . . ?
N21 C21 H21 118.8 . . ?
C22 C21 H21 118.8 . . ?
C21 C22 C23 119.4(3) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C22 C23 C24 118.2(3) . . ?
C22 C23 C26 118.8(3) . . ?
C24 C23 C26 122.9(3) . . ?
C25 C24 C23 118.7(3) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
N21 C25 C24 123.1(3) . . ?
N21 C25 H25 118.5 . . ?
C24 C25 H25 118.5 . . ?
O21 C26 N22 122.8(3) . . ?
O21 C26 C23 119.2(3) . . ?
N22 C26 C23 118.0(3) . . ?
C1 N1 Ni1 170.7(2) . . ?
C2 N2 Ni1 158.3(2) . . ?
C11 N11 C15 117.2(2) . . ?
C11 N11 Ni1 121.34(19) . . ?
C15 N11 Ni1 121.1(2) . . ?
C16 N12 H12A 120 . . ?
C16 N12 H12B 120 . . ?
H12A N12 H12B 120 . . ?
C25 N21 C21 118.2(2) . . ?
C25 N21 Ni1 121.21(19) . . ?
C21 N21 Ni1 120.56(19) . . ?
C26 N22 H22A 120 . . ?
C26 N22 H22B 120 . . ?
H22A N22 H22B 120 . . ?
C1 S1 Ni1 95.83(10) . 2_565 ?
C2 S2 Ni1 103.31(10) . 2 ?
N2 Ni1 N1 175.13(10) . . ?
N2 Ni1 N21 89.35(9) . . ?
N1 Ni1 N21 91.22(9) . . ?
N2 Ni1 N11 87.98(10) . . ?
N1 Ni1 N11 91.75(9) . . ?
N21 Ni1 N11 175.53(10) . . ?
N2 Ni1 S2 94.67(8) . 2 ?
N1 Ni1 S2 80.48(7) . 2 ?
N21 Ni1 S2 92.07(7) . 2 ?
N11 Ni1 S2 91.72(7) . 2 ?
N2 Ni1 S1 90.92(8) . 2_565 ?
N1 Ni1 S1 93.93(7) . 2_565 ?
N21 Ni1 S1 89.32(7) . 2_565 ?
N11 Ni1 S1 87.15(7) . 2_565 ?
S2 Ni1 S1 174.26(3) 2 2_565 ?
C102 C101 C107 121.1(3) . 2_666 ?
C102 C101 H101 119.5 . . ?
C107 C101 H101 119.5 2_666 . ?
C101 C102 C103 119.5(3) . . ?
C101 C102 H102 120.3 . . ?
C103 C102 H102 120.3 . . ?
C102 C103 C105 119.8(3) . 2_666 ?
C102 C103 C104 119.3(3) . . ?
C105 C103 C104 120.9(3) 2_666 . ?
O101 C104 C105 121.0(3) . . ?
O101 C104 C103 121.1(3) . . ?
C105 C104 C103 117.9(3) . . ?
C106 C105 C103 119.8(3) . 2_666 ?
C106 C105 C104 119.0(3) . . ?
C103 C105 C104 121.2(3) 2_666 . ?
C107 C106 C105 120.6(3) . . ?
C107 C106 H106 119.7 . . ?
C105 C106 H106 119.7 . . ?
C106 C107 C101 119.2(3) . 2_666 ?
C106 C107 H107 120.4 . . ?
C101 C107 H107 120.4 2_666 . ?

#===END


