# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_C:\1a.CIF
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            1a
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H30 Cl4 N6 Ni2 O2'
_chemical_formula_sum            'C24 H30 Cl4 N6 Ni2 O2'
_chemical_formula_weight         693.72

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   8.4860(14)
_cell_length_b                   14.430(2)
_cell_length_c                   11.5135(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.387(2)
_cell_angle_gamma                90.00
_cell_volume                     1403.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3869
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      28.30

_exptl_crystal_description       shard
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             712
_exptl_absorpt_coefficient_mu    1.757
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7651
_exptl_absorpt_correction_T_max  0.8012
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8711
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         28.43
_reflns_number_total             3237
_reflns_number_gt                2829
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'X-Seed (Atwood & Barbour, 2003)'
_computing_publication_material  'X-Seed (Atwood & Barbour, 2003)'

_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)+(0.0229P)²+0.7990P] 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_extinction_coef       ?
_refine_ls_number_reflns         3237
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0581
_refine_ls_wR_factor_gt          0.0553
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.51810(2) 0.965292(15) 0.857269(18) 0.00999(7) Uani 1 1 d . . .
Cl1 Cl 0.23778(5) 0.96550(3) 0.80728(4) 0.01444(10) Uani 1 1 d . . .
O1 O 0.76484(14) 0.97428(9) 0.92387(11) 0.0134(3) Uani 1 1 d . . .
N1 N 0.54561(17) 0.84242(11) 0.77472(13) 0.0161(3) Uani 1 1 d . . .
C1 C 0.4561(2) 0.77004(13) 0.80304(16) 0.0192(4) Uani 1 1 d . . .
H1 H 0.3713 0.7816 0.8494 0.023 Uiso 1 1 calc R . .
C1' C 0.4958(2) 1.10625(14) 0.67269(16) 0.0243(4) Uani 1 1 d . . .
H1' H 0.4179 1.1296 0.7191 0.029 Uiso 1 1 calc R . .
H1O H 0.757(3) 0.9978(18) 0.981(2) 0.033(7) Uiso 1 1 d . . .
Cl2 Cl 0.50940(5) 1.11184(3) 0.95779(3) 0.01195(9) Uani 1 1 d . . .
N2 N 0.56702(18) 1.02556(11) 0.70405(12) 0.0183(3) Uani 1 1 d . . .
C2 C 0.4812(3) 0.68043(15) 0.76829(18) 0.0296(5) Uani 1 1 d . . .
H2 H 0.4154 0.6311 0.7894 0.035 Uiso 1 1 calc R . .
C2' C 0.5302(3) 1.15651(17) 0.57677(18) 0.0381(6) Uani 1 1 d . . .
H2' H 0.4789 1.2138 0.5580 0.046 Uiso 1 1 calc R . .
N3 N 0.74378(19) 0.90446(14) 0.66705(14) 0.0282(4) Uani 1 1 d . . .
C3 C 0.6058(3) 0.66483(17) 0.70143(19) 0.0368(6) Uani 1 1 d . . .
H3 H 0.6301 0.6035 0.6790 0.044 Uiso 1 1 calc R . .
C3' C 0.6421(3) 1.1209(2) 0.50822(19) 0.0489(8) Uani 1 1 d . . .
H3' H 0.6699 1.1543 0.4420 0.059 Uiso 1 1 calc R . .
C4 C 0.6939(3) 0.73743(18) 0.66769(18) 0.0342(6) Uani 1 1 d . . .
H4 H 0.7780 0.7270 0.6203 0.041 Uiso 1 1 calc R . .
C4' C 0.7120(3) 1.0378(2) 0.53671(18) 0.0407(7) Uani 1 1 d . . .
H4' H 0.7870 1.0124 0.4893 0.049 Uiso 1 1 calc R . .
C5 C 0.6596(2) 0.82796(16) 0.70348(16) 0.0231(4) Uani 1 1 d . . .
C6 C 0.8966(2) 0.8842(2) 0.6209(2) 0.0519(8) Uani 1 1 d . . .
H6A H 0.8776 0.8617 0.5405 0.078 Uiso 1 1 calc R . .
H6B H 0.9530 0.8366 0.6692 0.078 Uiso 1 1 calc R . .
H6C H 0.9606 0.9408 0.6223 0.078 Uiso 1 1 calc R . .
C7 C 0.8632(2) 0.89443(13) 0.94766(16) 0.0179(4) Uani 1 1 d . . .
H7A H 0.8009 0.8447 0.9789 0.027 Uiso 1 1 calc R . .
H7B H 0.9518 0.9106 1.0049 0.027 Uiso 1 1 calc R . .
H7C H 0.9044 0.8734 0.8754 0.027 Uiso 1 1 calc R . .
C7C C 0.6727(2) 0.98959(17) 0.63648(16) 0.0255(5) Uani 1 1 d . . .


_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 N1 2.0355(15) . ?
Ni1 N2 2.0440(15) . ?
Ni1 O1 2.1651(13) . ?
Ni1 Cl1 2.3944(6) . ?
Ni1 Cl2 2.4152(6) . ?
Ni1 Cl2 2.4332(5) 3_677 ?
O1 C7 1.434(2) . ?
O1 H1O 0.75(2) . ?
N1 C5 1.342(2) . ?
N1 C1 1.349(2) . ?
C1 C2 1.376(3) . ?
C1 H1 0.9500 . ?
C1' N2 1.346(3) . ?
C1' C2' 1.375(3) . ?
C1' H1' 0.9500 . ?
Cl2 Ni1 2.4332(5) 3_677 ?
N2 C7C 1.345(3) . ?
C2 C3 1.384(3) . ?
C2 H2 0.9500 . ?
C2' C3' 1.389(4) . ?
C2' H2' 0.9500 . ?
N3 C7C 1.399(3) . ?
N3 C5 1.400(3) . ?
N3 C6 1.476(2) . ?
C3 C4 1.365(4) . ?
C3 H3 0.9500 . ?
C3' C4' 1.365(4) . ?
C3' H3' 0.9500 . ?
C4 C5 1.408(3) . ?
C4 H4 0.9500 . ?
C4' C7C 1.409(3) . ?
C4' H4' 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

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 Ni1 N2 85.77(6) . . ?
N1 Ni1 O1 93.90(5) . . ?
N2 Ni1 O1 90.70(6) . . ?
N1 Ni1 Cl1 92.51(4) . . ?
N2 Ni1 Cl1 94.00(5) . . ?
O1 Ni1 Cl1 172.32(4) . . ?
N1 Ni1 Cl2 175.19(4) . . ?
N2 Ni1 Cl2 93.37(5) . . ?
O1 Ni1 Cl2 81.37(4) . . ?
Cl1 Ni1 Cl2 92.277(16) . . ?
N1 Ni1 Cl2 91.99(5) . 3_677 ?
N2 Ni1 Cl2 173.61(5) . 3_677 ?
O1 Ni1 Cl2 83.48(4) . 3_677 ?
Cl1 Ni1 Cl2 92.073(16) . 3_677 ?
Cl2 Ni1 Cl2 88.363(19) . 3_677 ?
C7 O1 Ni1 123.09(11) . . ?
C7 O1 H1O 107.2(19) . . ?
Ni1 O1 H1O 99.8(19) . . ?
C5 N1 C1 118.80(17) . . ?
C5 N1 Ni1 122.79(14) . . ?
C1 N1 Ni1 118.01(12) . . ?
N1 C1 C2 123.5(2) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
N2 C1' C2' 123.2(2) . . ?
N2 C1' H1' 118.4 . . ?
C2' C1' H1' 118.4 . . ?
Ni1 Cl2 Ni1 91.637(19) . 3_677 ?
C7C N2 C1' 119.06(17) . . ?
C7C N2 Ni1 122.36(14) . . ?
C1' N2 Ni1 118.51(13) . . ?
C1 C2 C3 117.5(2) . . ?
C1 C2 H2 121.3 . . ?
C3 C2 H2 121.3 . . ?
C1' C2' C3' 118.0(2) . . ?
C1' C2' H2' 121.0 . . ?
C3' C2' H2' 121.0 . . ?
C7C N3 C5 123.21(16) . . ?
C7C N3 C6 117.1(2) . . ?
C5 N3 C6 116.2(2) . . ?
C4 C3 C2 120.1(2) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4' C3' C2' 119.6(2) . . ?
C4' C3' H3' 120.2 . . ?
C2' C3' H3' 120.2 . . ?
C3 C4 C5 119.7(2) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C3' C4' C7C 119.9(2) . . ?
C3' C4' H4' 120.0 . . ?
C7C C4' H4' 120.0 . . ?
N1 C5 N3 118.53(18) . . ?
N1 C5 C4 120.2(2) . . ?
N3 C5 C4 121.23(19) . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O1 C7 H7A 109.5 . . ?
O1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C7C N3 119.24(17) . . ?
N2 C7C C4' 120.2(2) . . ?
N3 C7C C4' 120.6(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 O1 C7 -28.01(13) . . . . ?
N2 Ni1 O1 C7 -113.81(13) . . . . ?
Cl2 Ni1 O1 C7 152.88(13) . . . . ?
Cl2 Ni1 O1 C7 63.55(12) 3_677 . . . ?
N2 Ni1 N1 C5 40.48(14) . . . . ?
O1 Ni1 N1 C5 -49.93(15) . . . . ?
Cl1 Ni1 N1 C5 134.31(14) . . . . ?
Cl2 Ni1 N1 C5 -133.53(14) 3_677 . . . ?
N2 Ni1 N1 C1 -146.85(14) . . . . ?
O1 Ni1 N1 C1 122.74(13) . . . . ?
Cl1 Ni1 N1 C1 -53.03(13) . . . . ?
Cl2 Ni1 N1 C1 39.14(13) 3_677 . . . ?
C5 N1 C1 C2 3.9(3) . . . . ?
Ni1 N1 C1 C2 -169.02(14) . . . . ?
N2 Ni1 Cl2 Ni1 -173.85(5) . . . 3_677 ?
O1 Ni1 Cl2 Ni1 -83.66(4) . . . 3_677 ?
Cl1 Ni1 Cl2 Ni1 92.010(16) . . . 3_677 ?
Cl2 Ni1 Cl2 Ni1 0.0 3_677 . . 3_677 ?
C2' C1' N2 C7C -2.8(3) . . . . ?
C2' C1' N2 Ni1 174.34(15) . . . . ?
N1 Ni1 N2 C7C -36.34(14) . . . . ?
O1 Ni1 N2 C7C 57.52(14) . . . . ?
Cl1 Ni1 N2 C7C -128.56(14) . . . . ?
Cl2 Ni1 N2 C7C 138.91(14) . . . . ?
N1 Ni1 N2 C1' 146.64(14) . . . . ?
O1 Ni1 N2 C1' -119.49(13) . . . . ?
Cl1 Ni1 N2 C1' 54.42(13) . . . . ?
Cl2 Ni1 N2 C1' -38.10(13) . . . . ?
N1 C1 C2 C3 0.4(3) . . . . ?
N2 C1' C2' C3' 1.1(3) . . . . ?
C1 C2 C3 C4 -3.1(3) . . . . ?
C1' C2' C3' C4' 0.9(3) . . . . ?
C2 C3 C4 C5 1.4(3) . . . . ?
C2' C3' C4' C7C -1.3(3) . . . . ?
C1 N1 C5 N3 175.04(16) . . . . ?
Ni1 N1 C5 N3 -12.3(2) . . . . ?
C1 N1 C5 C4 -5.6(3) . . . . ?
Ni1 N1 C5 C4 167.03(13) . . . . ?
C7C N3 C5 N1 -40.0(3) . . . . ?
C6 N3 C5 N1 161.61(17) . . . . ?
C7C N3 C5 C4 140.62(19) . . . . ?
C6 N3 C5 C4 -17.8(3) . . . . ?
C3 C4 C5 N1 3.0(3) . . . . ?
C3 C4 C5 N3 -177.64(18) . . . . ?
C1' N2 C7C N3 -178.26(16) . . . . ?
Ni1 N2 C7C N3 4.7(2) . . . . ?
C1' N2 C7C C4' 2.3(3) . . . . ?
Ni1 N2 C7C C4' -174.70(14) . . . . ?
C5 N3 C7C N2 44.3(3) . . . . ?
C6 N3 C7C N2 -157.55(17) . . . . ?
C5 N3 C7C C4' -136.30(19) . . . . ?
C6 N3 C7C C4' 21.9(3) . . . . ?
C3' C4' C7C N2 -0.3(3) . . . . ?
C3' C4' C7C N3 -179.74(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.914
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.065

#==============================================================================
_iucr_refine_instruction_details 
;
REM  1a in P2(1)/n
REM R1 =  0.0261 for   2829 Fo > 4sig(Fo)  and  0.0317 for all   3237 data
REM    174 parameters refined using      0 restraints
REM Highest difference peak  0.818,  deepest hole -0.309,  1-sigma level  0.071
REM  SOLVE1 in P2(1)/n
REM R1 =  0.0249 for   2829 Fo > 4sig(Fo)  and  0.0305 for all   3237 data
REM    178 parameters refined using      0 restraints
REM Highest difference peak  0.358,  deepest hole -0.314,  1-sigma level  0.065
REM  SOLVE1 in P2(1)/n
REM R1 =  0.0249 for   2829 Fo > 4sig(Fo)  and  0.0305 for all   3237 data
REM    178 parameters refined using      0 restraints
REM Highest difference peak  0.358,  deepest hole -0.314,  1-sigma level  0.065
REM  SOLVE1 in P2(1)/n
REM R1 =  0.0249 for   2829 Fo > 4sig(Fo)  and  0.0305 for all   3237 data
REM    178 parameters refined using      0 restraints
REM Highest difference peak  0.358,  deepest hole -0.314,  1-sigma level  0.065
REM  SOLVE1 in P2(1)/n
REM R1 =  0.0249 for   2829 Fo > 4sig(Fo)  and  0.0305 for all   3237 data
REM    178 parameters refined using      0 restraints
REM Highest difference peak  0.358,  deepest hole -0.314,  1-sigma level  0.065
REM  SOLVE1 in P2(1)/n
REM R1 =  0.0724 for   2829 Fo > 4sig(Fo)  and  0.0806 for all   3237 data
REM     78 parameters refined using      0 restraints
REM Highest difference peak  2.375,  deepest hole -1.167,  1-sigma level  0.187
REM  SOLVE1 in P2(1)/n
REM R1 =  0.0299 for   2829 Fo > 4sig(Fo)  and  0.0355 for all   3237 data
REM    173 parameters refined using      0 restraints
REM Highest difference peak  0.740,  deepest hole -0.924,  1-sigma level  0.085
REM  SOLVE1 in P2(1)/n
REM R1 =  0.0249 for   2829 Fo > 4sig(Fo)  and  0.0305 for all   3237 data
REM    178 parameters refined using      0 restraints
REM Highest difference peak  0.358,  deepest hole -0.314,  1-sigma level  0.065
REM  SOLVE1 in P2(1)/n
REM R1 =  0.0249 for   2829 Fo > 4sig(Fo)  and  0.0305 for all   3237 data
REM    178 parameters refined using      0 restraints
REM Highest difference peak  0.358,  deepest hole -0.314,  1-sigma level  0.065
TITL SOLVE1 in P2(1)/n
CELL 0.71073 8.4860 14.4304 11.5135 90.000 95.387 90.000
ZERR 1.0000 0.0014 0.0024 0.0019 0.000 0.002 0.000
LATT 1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H N CL NI O
UNIT 48 60 12 8 4 4
MERG 2
FMAP 2
GRID
PLAN 20
TEMP -173
SIZE 0.132 0.149 0.161
HTAB
BOND $H
CONF
L.S. 4
ACTA 50
WGHT    0.022900    0.799000
FVAR       0.14125
NI1   5    0.518102    0.965292    0.857269    11.00000    0.01055    0.01095 =
         0.00876   -0.00148    0.00247   -0.00151
CL1   4    0.237777    0.965496    0.807278    11.00000    0.01134    0.01583 =
         0.01593   -0.00232    0.00013   -0.00029
O1    6    0.764843    0.974280    0.923868    11.00000    0.01298    0.01513 =
         0.01206   -0.00138    0.00137    0.00050
N1    3    0.545614    0.842421    0.774716    11.00000    0.01259    0.01969 =
         0.01563   -0.00883   -0.00118    0.00297
C1    1    0.456121    0.770038    0.803043    11.00000    0.02094    0.01564 =
         0.01964   -0.00666   -0.00592    0.00209
AFIX  43
H1    2    0.371349    0.781552    0.849431    11.00000   -1.20000
AFIX   0
C1'   1    0.495777    1.106247    0.672688    11.00000    0.02985    0.02640 =
         0.01488    0.00454   -0.00753   -0.01569
AFIX  43
H1'   2    0.417897    1.129646    0.719090    11.00000   -1.20000
AFIX   0
H1O   2    0.756514    0.997784    0.981323    11.00000    0.03346
CL2   4    0.509401    1.111840    0.957792    11.00000    0.01457    0.00966 =
         0.01194    0.00010    0.00290   -0.00192
N2    3    0.567019    1.025562    0.704052    11.00000    0.01797    0.02782 =
         0.00884   -0.00085   -0.00040   -0.01140
C2    1    0.481160    0.680426    0.768289    11.00000    0.04122    0.01808 =
         0.02572   -0.00784   -0.01641    0.00766
AFIX  43
H2    2    0.415354    0.631126    0.789397    11.00000   -1.20000
AFIX   0
C2'   1    0.530155    1.156505    0.576772    11.00000    0.05258    0.04001 =
         0.01778    0.01254   -0.01735   -0.03220
AFIX  43
H2'   2    0.478895    1.213821    0.557959    11.00000   -1.20000
AFIX   0
N3    3    0.743777    0.904460    0.667047    11.00000    0.01188    0.05707 =
         0.01633   -0.01604    0.00569   -0.00307
C3    1    0.605806    0.664826    0.701434    11.00000    0.04711    0.03033 =
         0.02782   -0.01893   -0.02342    0.02456
AFIX  43
H3    2    0.630064    0.603491    0.678994    11.00000   -1.20000
AFIX   0
C3'   1    0.642104    1.120930    0.508222    11.00000    0.06014    0.07329 =
         0.01140    0.00951   -0.00622   -0.05348
AFIX  43
H3'   2    0.669851    1.154263    0.441964    11.00000   -1.20000
AFIX   0
C4    1    0.693933    0.737431    0.667695    11.00000    0.02457    0.05441 =
         0.02080   -0.02296   -0.01200    0.02614
AFIX  43
H4    2    0.777993    0.726960    0.620302    11.00000   -1.20000
AFIX   0
C4'   1    0.711955    1.037768    0.536707    11.00000    0.03598    0.07618 =
         0.01096   -0.00784    0.00679   -0.03809
AFIX  43
H4'   2    0.786985    1.012383    0.489318    11.00000   -1.20000
AFIX   0
C5    1    0.659643    0.827958    0.703483    11.00000    0.01286    0.04058 =
         0.01493   -0.01448   -0.00433    0.00585
C6    1    0.896599    0.884184    0.620880    11.00000    0.01539    0.11018 =
         0.03157   -0.03540    0.00996   -0.00657
AFIX 137
H6A   2    0.877569    0.861728    0.540457    11.00000   -1.50000
H6B   2    0.953033    0.836607    0.669219    11.00000   -1.50000
H6C   2    0.960643    0.940756    0.622318    11.00000   -1.50000
AFIX   0
C7    1    0.863248    0.894432    0.947661    11.00000    0.01415    0.01925 =
         0.02007   -0.00143    0.00071    0.00242
AFIX 137
H7A   2    0.800855    0.844715    0.978926    11.00000   -1.50000
H7B   2    0.951774    0.910575    1.004931    11.00000   -1.50000
H7C   2    0.904352    0.873446    0.875382    11.00000   -1.50000
AFIX   0
C7C   1    0.672685    0.989587    0.636478    11.00000    0.01790    0.04823 =
         0.01030   -0.00734    0.00090   -0.01886
HKLF 4
 
REM  SOLVE1 in P2(1)/n
REM R1 =  0.0249 for   2829 Fo > 4sig(Fo)  and  0.0305 for all   3237 data
REM    178 parameters refined using      0 restraints
 
END  
     
WGHT      0.0229      0.7990 
REM Highest difference peak  0.358,  deepest hole -0.314,  1-sigma level  0.065
Q1    1   0.5216  0.6823  0.7162  11.00000  0.05    0.36
Q2    1   0.6601  0.7832  0.6727  11.00000  0.05    0.33
Q3    1   0.8292  0.8441  0.9204  11.00000  0.05    0.32
Q4    1   0.9513  0.8601  0.6617  11.00000  0.05    0.30
Q5    1   0.6206  0.7093  0.6605  11.00000  0.05    0.29
Q6    1   0.5596  1.0000  0.7565  11.00000  0.05    0.28
Q7    1   0.8423  0.8629  1.0187  11.00000  0.05    0.27
Q8    1   0.4760  0.7166  0.7909  11.00000  0.05    0.27
Q9    1   0.5039  0.8035  0.7748  11.00000  0.05    0.27
Q10   1   0.9702  0.9073  0.9400  11.00000  0.05    0.27
Q11   1   0.6408  1.0266  0.6802  11.00000  0.05    0.26
Q12   1   0.7212  0.9568  0.6784  11.00000  0.05    0.26
Q13   1   0.6992  1.0903  0.5375  11.00000  0.05    0.26
Q14   1   0.8719  0.8852  0.5227  11.00000  0.05    0.25
Q15   1   0.6760  0.9628  0.8918  11.00000  0.05    0.25
Q16   1   0.7574  0.7562  0.6571  11.00000  0.05    0.24
Q17   1   0.6635  1.0146  0.5878  11.00000  0.05    0.24
Q18   1   0.6774  0.8631  0.6666  11.00000  0.05    0.23
Q19   1   0.7551  1.0215  0.5378  11.00000  0.05    0.23
Q20   1   0.5992  0.8324  0.7377  11.00000  0.05    0.23
;
_database_code_depnum_ccdc_archive 'CCDC 981834'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_c:\1e-A.cif
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C13 H16 N3), Cl4 Ni, H2 O'
_chemical_formula_sum            'C26 H34 Cl4 N6 Ni O'
_chemical_formula_weight         647.10

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   21.751(4)
_cell_length_b                   11.949(2)
_cell_length_c                   13.415(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 123.276(2)
_cell_angle_gamma                90.00
_cell_volume                     2915.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2911
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      28.41

_exptl_crystal_description       shard
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1344
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8028
_exptl_absorpt_correction_T_max  0.8983
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            8948
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         28.43
_reflns_number_total             3379
_reflns_number_gt                2794
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SAINT (Bruker 2002)'
_computing_cell_refinement       'SAINT (Bruker 2002)'
_computing_data_reduction        'SAINT (Bruker 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'X-Seed (Atwood & Barbour, 2003)'
_computing_publication_material  'X-Seed (Atwood & Barbour, 2003)'

_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)+(0.0299P)²+1.7343P] 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_extinction_coef       ?
_refine_ls_number_reflns         3379
_refine_ls_number_parameters     184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0718
_refine_ls_wR_factor_gt          0.0674
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.0000 0.24608(3) 0.2500 0.01559(10) Uani 1 2 d S . .
N1 N 0.29263(8) -0.01440(13) 0.37997(13) 0.0159(3) Uani 1 1 d . . .
N2 N 0.18408(8) -0.11870(13) 0.30104(14) 0.0203(3) Uani 1 1 d . . .
C3 C 0.33448(10) 0.07927(15) 0.41832(16) 0.0174(4) Uani 1 1 d . . .
C4 C 0.21980(10) -0.01669(16) 0.33545(15) 0.0185(4) Uani 1 1 d . . .
N5 N 0.29204(8) -0.22533(12) 0.38885(13) 0.0163(3) Uani 1 1 d . . .
C6 C 0.33019(10) -0.32150(15) 0.43282(16) 0.0173(4) Uani 1 1 d . . .
C7 C 0.22021(11) -0.41729(17) 0.38135(17) 0.0238(4) Uani 1 1 d . . .
H7 H 0.1954 -0.4841 0.3778 0.029 Uiso 1 1 calc R . .
C8 C 0.18512(11) 0.08441(17) 0.32788(17) 0.0228(4) Uani 1 1 d . . .
H8 H 0.1340 0.0865 0.2970 0.027 Uiso 1 1 calc R . .
C9 C 0.21984(10) -0.22275(16) 0.34388(16) 0.0187(4) Uani 1 1 d . . .
C10 C 0.29534(11) -0.42022(16) 0.42841(16) 0.0213(4) Uani 1 1 d . . .
H10 H 0.3221 -0.4883 0.4568 0.026 Uiso 1 1 calc R . .
C11 C 0.18145(10) -0.31848(17) 0.33989(17) 0.0223(4) Uani 1 1 d . . .
H11 H 0.1305 -0.3154 0.3096 0.027 Uiso 1 1 calc R . .
C12 C 0.41392(10) 0.06426(16) 0.46500(17) 0.0204(4) Uani 1 1 d . . .
H12A H 0.4372 0.0186 0.5375 0.031 Uiso 1 1 calc R . .
H12B H 0.4380 0.1376 0.4834 0.031 Uiso 1 1 calc R . .
H12C H 0.4188 0.0267 0.4047 0.031 Uiso 1 1 calc R . .
C13 C 0.22639(11) 0.18041(17) 0.36597(17) 0.0242(4) Uani 1 1 d . . .
H13 H 0.2033 0.2494 0.3613 0.029 Uiso 1 1 calc R . .
C14 C 0.41106(10) -0.31381(16) 0.48535(18) 0.0221(4) Uani 1 1 d . . .
H14A H 0.4193 -0.2874 0.4245 0.033 Uiso 1 1 calc R . .
H14B H 0.4335 -0.3878 0.5136 0.033 Uiso 1 1 calc R . .
H14C H 0.4333 -0.2612 0.5524 0.033 Uiso 1 1 calc R . .
C15 C 0.30144(11) 0.17932(16) 0.41139(16) 0.0215(4) Uani 1 1 d . . .
H15 H 0.3292 0.2467 0.4371 0.026 Uiso 1 1 calc R . .
C17 C 0.10281(10) -0.11700(19) 0.23067(18) 0.0286(5) Uani 1 1 d . . .
H17A H 0.0858 -0.1131 0.2847 0.043 Uiso 1 1 calc R . .
H17B H 0.0838 -0.1853 0.1825 0.043 Uiso 1 1 calc R . .
H17C H 0.0850 -0.0515 0.1781 0.043 Uiso 1 1 calc R . .
Cl3 Cl 0.08167(2) 0.36833(4) 0.25443(4) 0.01878(11) Uani 1 1 d . . .
Cl2 Cl 0.04505(3) 0.12624(4) 0.40501(4) 0.02293(12) Uani 1 1 d . . .
O3 O 0.0000 0.59785(19) 0.2500 0.0384(6) Uani 1 2 d S . .
H6 H 0.0311(17) 0.542(3) 0.245(3) 0.095(12) Uiso 1 1 d . . .
H1 H 0.3121(13) -0.080(2) 0.387(2) 0.040(7) Uiso 1 1 d . . .


_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 Cl2 2.2581(6) 2 ?
Ni1 Cl2 2.2581(6) . ?
Ni1 Cl3 2.2753(5) . ?
Ni1 Cl3 2.2753(5) 2 ?
N1 C4 1.352(2) . ?
N1 C3 1.354(2) . ?
N1 H1 0.87(2) . ?
N2 C4 1.382(2) . ?
N2 C9 1.411(2) . ?
N2 C17 1.478(2) . ?
C3 C15 1.372(3) . ?
C3 C12 1.491(3) . ?
C4 C8 1.398(3) . ?
N5 C9 1.338(2) . ?
N5 C6 1.349(2) . ?
C6 C10 1.386(3) . ?
C6 C14 1.496(2) . ?
C7 C11 1.378(3) . ?
C7 C10 1.392(3) . ?
C7 H7 0.9500 . ?
C8 C13 1.371(3) . ?
C8 H8 0.9500 . ?
C9 C11 1.400(3) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C15 1.395(3) . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
O3 H6 0.98(3) . ?

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
Cl2 Ni1 Cl2 101.29(3) 2 . ?
Cl2 Ni1 Cl3 111.668(18) 2 . ?
Cl2 Ni1 Cl3 116.424(18) . . ?
Cl2 Ni1 Cl3 116.423(18) 2 2 ?
Cl2 Ni1 Cl3 111.668(18) . 2 ?
Cl3 Ni1 Cl3 100.12(3) . 2 ?
C4 N1 C3 124.41(16) . . ?
C4 N1 H1 114.2(16) . . ?
C3 N1 H1 121.2(16) . . ?
C4 N2 C9 123.92(15) . . ?
C4 N2 C17 117.22(16) . . ?
C9 N2 C17 118.11(16) . . ?
N1 C3 C15 118.48(17) . . ?
N1 C3 C12 116.29(15) . . ?
C15 C3 C12 125.23(17) . . ?
N1 C4 N2 118.24(16) . . ?
N1 C4 C8 117.99(17) . . ?
N2 C4 C8 123.77(17) . . ?
C9 N5 C6 120.32(16) . . ?
N5 C6 C10 121.03(17) . . ?
N5 C6 C14 115.83(16) . . ?
C10 C6 C14 123.14(17) . . ?
C11 C7 C10 120.69(18) . . ?
C11 C7 H7 119.7 . . ?
C10 C7 H7 119.7 . . ?
C13 C8 C4 118.62(18) . . ?
C13 C8 H8 120.7 . . ?
C4 C8 H8 120.7 . . ?
N5 C9 C11 121.75(17) . . ?
N5 C9 N2 116.88(16) . . ?
C11 C9 N2 121.36(17) . . ?
C6 C10 C7 118.46(18) . . ?
C6 C10 H10 120.8 . . ?
C7 C10 H10 120.8 . . ?
C7 C11 C9 117.68(18) . . ?
C7 C11 H11 121.2 . . ?
C9 C11 H11 121.2 . . ?
C3 C12 H12A 109.5 . . ?
C3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C8 C13 C15 121.67(18) . . ?
C8 C13 H13 119.2 . . ?
C15 C13 H13 119.2 . . ?
C6 C14 H14A 109.5 . . ?
C6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C3 C15 C13 118.82(18) . . ?
C3 C15 H15 120.6 . . ?
C13 C15 H15 120.6 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N1 C3 C15 -0.4(3) . . . . ?
C4 N1 C3 C12 179.70(16) . . . . ?
C3 N1 C4 N2 -179.16(16) . . . . ?
C3 N1 C4 C8 0.3(3) . . . . ?
C9 N2 C4 N1 22.3(3) . . . . ?
C17 N2 C4 N1 -167.88(16) . . . . ?
C9 N2 C4 C8 -157.16(18) . . . . ?
C17 N2 C4 C8 12.7(3) . . . . ?
C9 N5 C6 C10 2.5(3) . . . . ?
C9 N5 C6 C14 -177.59(16) . . . . ?
N1 C4 C8 C13 -0.1(3) . . . . ?
N2 C4 C8 C13 179.28(17) . . . . ?
C6 N5 C9 C11 -0.5(3) . . . . ?
C6 N5 C9 N2 179.22(16) . . . . ?
C4 N2 C9 N5 -21.6(3) . . . . ?
C17 N2 C9 N5 168.65(16) . . . . ?
C4 N2 C9 C11 158.12(17) . . . . ?
C17 N2 C9 C11 -11.7(3) . . . . ?
N5 C6 C10 C7 -2.3(3) . . . . ?
C14 C6 C10 C7 177.77(17) . . . . ?
C11 C7 C10 C6 0.2(3) . . . . ?
C10 C7 C11 C9 1.7(3) . . . . ?
N5 C9 C11 C7 -1.6(3) . . . . ?
N2 C9 C11 C7 178.71(17) . . . . ?
C4 C8 C13 C15 0.1(3) . . . . ?
N1 C3 C15 C13 0.4(3) . . . . ?
C12 C3 C15 C13 -179.74(17) . . . . ?
C8 C13 C15 C3 -0.3(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.919
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.066

#==============================================================================
_iucr_refine_instruction_details 
;
REM  solve1 in C2/c
REM R1 =  0.0319 for   2794 Fo > 4sig(Fo)  and  0.0420 for all   3382 data
REM    184 parameters refined using      0 restraints
REM Highest difference peak  0.382,  deepest hole -0.383,  1-sigma level  0.067
REM  solve1 in C2/c
REM R1 =  0.0311 for   2794 Fo > 4sig(Fo)  and  0.0412 for all   3379 data
REM    185 parameters refined using      0 restraints
REM Highest difference peak  0.349,  deepest hole -0.289,  1-sigma level  0.066
REM  solve1 in C2/c
REM R1 =  0.0310 for   2794 Fo > 4sig(Fo)  and  0.0412 for all   3379 data
REM    185 parameters refined using      0 restraints
REM Highest difference peak  0.352,  deepest hole -0.289,  1-sigma level  0.066
REM  solve1 in C2/c
REM R1 =  0.0310 for   2794 Fo > 4sig(Fo)  and  0.0412 for all   3379 data
REM    185 parameters refined using      0 restraints
REM Highest difference peak  0.352,  deepest hole -0.289,  1-sigma level  0.066
REM  solve1 in C2/c
REM R1 =  0.0310 for   2794 Fo > 4sig(Fo)  and  0.0412 for all   3379 data
REM    184 parameters refined using      0 restraints
REM Highest difference peak  0.352,  deepest hole -0.290,  1-sigma level  0.066
TITL solve1 in C2/c
CELL 0.71073 21.7511 11.9490 13.4154 90.000 123.276 90.000
ZERR 4.0000 0.0036 0.0020 0.0022 0.000 0.002 0.000
LATT 7
SYMM -X, Y, 0.5-Z
SFAC C H N CL NI O
UNIT 104 136 24 16 4 4
MERG 2
FMAP 2
GRID
PLAN 20
TEMP -173
SIZE 0.103 0.154 0.216
OMIT     0 4 3
OMIT     1 1 0
OMIT     -17 9 3
BOND $H
HTAB
CONF
L.S. 20
ACTA 50
WGHT    0.029900    1.734300
FVAR       0.05717
NI1   5    0.000000    0.246083    0.250000    10.50000    0.01585    0.01113 =
         0.02276    0.00000    0.01248    0.00000
N1    3    0.292632   -0.014400    0.379971    11.00000    0.01500    0.01861 =
         0.01541    0.00354    0.00912    0.00521
N2    3    0.184079   -0.118705    0.301036    11.00000    0.01131    0.03046 =
         0.01746    0.00197    0.00689    0.00254
C3    1    0.334482    0.079271    0.418319    11.00000    0.02149    0.01977 =
         0.01239    0.00165    0.01014    0.00348
C4    1    0.219804   -0.016687    0.335448    11.00000    0.01742    0.02763 =
         0.01117    0.00476    0.00835    0.00508
N5    3    0.292043   -0.225333    0.388847    11.00000    0.01422    0.02061 =
         0.01476   -0.00137    0.00848   -0.00016
C6    1    0.330193   -0.321502    0.432819    11.00000    0.01914    0.02109 =
         0.01484   -0.00116    0.01142   -0.00010
C7    1    0.220214   -0.417292    0.381355    11.00000    0.02863    0.02765 =
         0.01877   -0.00886    0.01525   -0.01376
AFIX  43
H7    2    0.195403   -0.484102    0.377788    11.00000   -1.20000
AFIX   0
C8    1    0.185120    0.084412    0.327883    11.00000    0.01888    0.03389 =
         0.01790    0.00735    0.01150    0.01242
AFIX  43
H8    2    0.134015    0.086536    0.296986    11.00000   -1.20000
AFIX   0
C9    1    0.219842   -0.222754    0.343879    11.00000    0.01601    0.02745 =
         0.01269   -0.00314    0.00798   -0.00215
C10   1    0.295338   -0.420218    0.428409    11.00000    0.02812    0.01994 =
         0.01744   -0.00230    0.01360   -0.00319
AFIX  43
H10   2    0.322091   -0.488308    0.456838    11.00000   -1.20000
AFIX   0
C11   1    0.181452   -0.318478    0.339886    11.00000    0.01571    0.03350 =
         0.01716   -0.00536    0.00869   -0.00720
AFIX  43
H11   2    0.130455   -0.315443    0.309647    11.00000   -1.20000
AFIX   0
C12   1    0.413922    0.064259    0.464997    11.00000    0.01720    0.02069 =
         0.02274   -0.00170    0.01062    0.00000
AFIX 137
H12A  2    0.437247    0.018585    0.537532    11.00000   -1.50000
H12B  2    0.437962    0.137589    0.483448    11.00000   -1.50000
H12C  2    0.418778    0.026736    0.404694    11.00000   -1.50000
AFIX   0
C13   1    0.226387    0.180411    0.365973    11.00000    0.02921    0.02642 =
         0.01911    0.00649    0.01467    0.01389
AFIX  43
H13   2    0.203270    0.249437    0.361309    11.00000   -1.20000
AFIX   0
C14   1    0.411059   -0.313807    0.485351    11.00000    0.02036    0.02065 =
         0.02702    0.00198    0.01415    0.00236
AFIX 137
H14A  2    0.419339   -0.287371    0.424482    11.00000   -1.50000
H14B  2    0.433464   -0.387811    0.513601    11.00000   -1.50000
H14C  2    0.433341   -0.261197    0.552379    11.00000   -1.50000
AFIX   0
C15   1    0.301437    0.179315    0.411394    11.00000    0.02754    0.02089 =
         0.01760    0.00290    0.01330    0.00583
AFIX  43
H15   2    0.329182    0.246672    0.437082    11.00000   -1.20000
AFIX   0
C17   1    0.102808   -0.117002    0.230672    11.00000    0.01189    0.04403 =
         0.02464    0.00305    0.00673    0.00151
AFIX 137
H17A  2    0.085771   -0.113124    0.284735    11.00000   -1.50000
H17B  2    0.083817   -0.185266    0.182525    11.00000   -1.50000
H17C  2    0.084957   -0.051486    0.178110    11.00000   -1.50000
AFIX   0
CL3   4    0.081667    0.368327    0.254426    11.00000    0.01401    0.01755 =
         0.02390    0.00221    0.00983   -0.00092
CL2   4    0.045047    0.126239    0.405008    11.00000    0.02444    0.01901 =
         0.02947    0.00703    0.01744    0.00444
O3    6    0.000000    0.597847    0.250000    10.50000    0.04265    0.02231 =
         0.04981    0.00000    0.02505    0.00000
H6    2    0.031120    0.541852    0.244733    11.00000    0.09489
H1    2    0.312091   -0.080070    0.387224    11.00000    0.04001
HKLF 4
 
REM  solve1 in C2/c
REM R1 =  0.0310 for   2794 Fo > 4sig(Fo)  and  0.0412 for all   3379 data
REM    184 parameters refined using      0 restraints
 
END  
     
WGHT      0.0299      1.7343 
REM Highest difference peak  0.352,  deepest hole -0.290,  1-sigma level  0.066
Q1    1   0.3127 -0.3720  0.4450  11.00000  0.05    0.35
Q2    1   0.3719 -0.3129  0.4546  11.00000  0.05    0.29
Q3    1   0.1996  0.0385  0.3212  11.00000  0.05    0.28
Q4    1   0.2080 -0.3572  0.3759  11.00000  0.05    0.28
Q5    1   0.3010 -0.2729  0.3935  11.00000  0.05    0.28
Q6    1   0.3014  0.0373  0.3637  11.00000  0.05    0.27
Q7    1   0.0020  0.3404  0.1972  11.00000  0.05    0.25
Q8    1   0.0787  0.1232  0.3615  11.00000  0.05    0.25
Q9    1   0.3745  0.0703  0.4501  11.00000  0.05    0.25
Q10   1   0.3100  0.1360  0.3814  11.00000  0.05    0.25
Q11   1   0.0387  0.2634  0.2187  11.00000  0.05    0.25
Q12   1   0.1515 -0.1069  0.2839  11.00000  0.05    0.24
Q13   1   0.1991 -0.2836  0.3185  11.00000  0.05    0.23
Q14   1   0.2594 -0.2272  0.3618  11.00000  0.05    0.23
Q15   1   0.2073 -0.4828  0.4451  11.00000  0.05    0.23
Q16   1   0.2554 -0.0115  0.3609  11.00000  0.05    0.23
Q17   1   0.2040 -0.2589  0.3675  11.00000  0.05    0.23
Q18   1   0.2039 -0.1783  0.3220  11.00000  0.05    0.23
Q19   1   0.0577  0.1998  0.3612  11.00000  0.05    0.22
Q20   1   0.0732  0.4560  0.1955  11.00000  0.05    0.22
;
#======================================================================

_database_code_depnum_ccdc_archive 'CCDC 981835'
