data_ras1515SN 
_audit_creation_date        "15-06-22"
_audit_creation_method CRYSTALS_ver_14.40

_audit_update_record                    
; 
2015-06-22 - Report on C26 H36 Cl2 N4 Ni O6
             by Anthony C. Willis 
             for Rasoul Vafazadeh and Zahra Mansouri
2015-06-22 - passes checkcif tests with minor warnings 
;  


_oxford_structure_analysis_title  'Z:\ras1515SN\Tony_ras1515SN_data At 16:15 on'
_chemical_name_systematic         ?
_chemical_melting_point           ?

_cell_length_a                     7.3033(1)
_cell_length_b                    19.2677(1)
_cell_length_c                    20.4218(1)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      2873.71(4)
 
_symmetry_cell_setting            'orthorhombic' 
_symmetry_space_group_name_H-M    'P b c a ' 
_symmetry_space_group_name_Hall   '-P 2ac 2ab ' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-x+1/2,y+1/2,z'
 'x+1/2,-y+1/2,-z'
 'x,-y+1/2,z+1/2'
 '-x,y+1/2,-z+1/2'
 '-x+1/2,-y,z+1/2'
 'x+1/2,y,-z+1/2'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0181   0.0091   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Cl      0.3639   0.7018  11.4604   0.0104   7.1964   1.1662   6.2556  18.5194
   1.6455  47.7784  -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 N       0.0311   0.0180  12.2126   0.0057   3.1322   9.8933   2.0125  28.9975
   1.1663   0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Ni     -3.0029   0.5091  12.8376   3.8785   7.2920   0.2565   4.4438  12.1763
   2.3800  66.3421   1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0492   0.0322   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    4

# Given Formula = C26 H38 Cl2 N4 Ni1 O6 
# Dc =      1.46 Fooo =   1320.00 Mu =     30.79 M =    316.11
# Found Formula = C26 H36 Cl2 N4 Ni1 O6 
# Dc =      1.46 FOOO =   1320.00 Mu =     30.79 M =    315.11

_chemical_formula_sum             'C26 H36 Cl2 N4 Ni O6'
_chemical_formula_moiety          'C26 H36 N4 Ni O6 2+, (Cl -)2'
_chemical_compound_source                ' Yazd University '
_chemical_formula_weight            630.21
 
 
_cell_measurement_reflns_used        20016
_cell_measurement_theta_min              4
_cell_measurement_theta_max             72
_cell_measurement_temperature          150
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_min           0.107 
_exptl_crystal_size_mid           0.119 
_exptl_crystal_size_max           0.220 
 
_exptl_crystal_density_diffrn     1.457 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1320 
_exptl_absorpt_coefficient_mu     3.079 
 
# Sheldrick geometric approximatio 0.69 0.72 
_exptl_absorpt_correction_type    multi-scan 


_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_correction_T_min   0.64 
_exptl_absorpt_correction_T_max   0.72 

_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2'  
_diffrn_radiation_source 'Supernova (Cu) X-ray Source'    
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'mirror' 
_diffrn_radiation_type            'Cu K\a'
_diffrn_radiation_wavelength           1.54184
_diffrn_measurement_method        \w 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
;
_computing_cell_refinement    'CrysAlisPro (Agilent Technologies, 2015)'
_computing_data_reduction     'CrysAlisPro (Agilent Technologies, 2015)'
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'PLATON (Spek, 2008)' 

 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        150
_diffrn_reflns_number             42463 
_reflns_number_total              2823 
_diffrn_reflns_av_R_equivalents   0.036 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 2823 
# Theoretical number of reflections is about 5690 
 
 
_diffrn_reflns_theta_min          4.590 
_diffrn_reflns_theta_max          72.417 
_diffrn_measured_fraction_theta_max 0.998 
 
_diffrn_reflns_theta_full         72.417 
_diffrn_measured_fraction_theta_full 0.998 
 
 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        6 
_diffrn_reflns_limit_k_min        -23 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        -25 
_diffrn_reflns_limit_l_max        25 
_reflns_limit_h_min               0 
_reflns_limit_h_max               9 
_reflns_limit_k_min               0 
_reflns_limit_k_max               23 
_reflns_limit_l_min               0 
_reflns_limit_l_max               25 
 
_oxford_diffrn_Wilson_B_factor    1.76 
_oxford_diffrn_Wilson_scale       0.37 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.25 
_refine_diff_density_max          0.29 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-10.0\s(I)
_refine_ls_number_reflns          2823 
_refine_ls_number_restraints      0 
_refine_ls_number_parameters      232 
_oxford_refine_ls_R_factor_ref    0.0290 
_refine_ls_wR_factor_ref          0.0723 
_refine_ls_goodness_of_fit_ref    1.0222 
_refine_ls_shift/su_max           0.0079388 
_refine_ls_shift/su_mean          0.0003581 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         2823 
_refine_ls_R_factor_all           0.0290 
_refine_ls_wR_factor_all          0.0723 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0\s(I)
_reflns_number_gt                 2777 
_refine_ls_R_factor_gt            0.0285 
_refine_ls_wR_factor_gt           0.0719 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     refxyz         #undef, noref, refall,
                                              # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 2.10P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;



# 1. SUBMISSION DETAILS                                                        
_publ_requested_journal               ' test ' 
_publ_requested_category               fm  
_publ_contact_author_name             ' Anthony C. Willis ' 
 
_publ_contact_author_address 
; 
Research School of Chemistry, 
Australian National University, 
Canberra, A. C. T. 2601, Australia 
; 
_publ_contact_letter 
; 
    ENTER TEXT OF LETTER 
; 
 
_publ_requested_coeditor_name          ? 
_publ_contact_author_phone            ' 61 2 6125 4109 ' 
_publ_contact_author_fax              ' 61 2 6125 0750 ' 
_publ_contact_author_email            ' Anthony.Willis@anu.edu.au ' 
                                                                              
#=============================================================================
# 2. PROCESSING SUMMARY (IUCr Office Use Only)                                
_journal_date_recd_electronic     ?                                           
_journal_date_to_coeditor         ?                                           
_journal_date_from_coeditor       ?                                           
_journal_date_accepted            ?                                           
_journal_date_printers_first      ?                                           
_journal_date_printers_final      ?                                           
_journal_date_proofs_out          ?                                           
_journal_date_proofs_in           ?                                           
_journal_coeditor_name            ?                                           
_journal_coeditor_code            ?                                           
_journal_coeditor_notes                                                       
;                                                                             
                                  ?                                           
;                                                                             
_journal_techeditor_code          ?                                           
_journal_techeditor_notes                                                     
;                                                                             
                                  ?                                           
;                                                                             
_journal_coden_ASTM               ?                                           
_journal_name_full                ?                                           
_journal_year                     ?                                           
_journal_volume                   ?                                           
_journal_issue                    ?                                           
_journal_page_first               ?                                           
_journal_page_last                ?                                           
_journal_suppl_publ_number        ?                                           
_journal_suppl_publ_pages         ?                                           
#=============================================================================
# 3. TITLE AND AUTHOR LIST                                                    
_publ_section_title                                                           
;                                                                             
Crystal structure of 
[Ni(C~12~H~14~N~2~O~2~)~2~(CH~3~OH)~2~]Cl~2~
--- ras1515SN  
;                                                                             
# The loop structure below should contain the names and addresses of all      
# authors, in the required order of publication. Repeat as necessary.         
loop_ 
_publ_author_name 
_publ_author_address 
' Zahra Mansouri ' 
; 
Department of Chemistry, 
Yazd University, 
Yazd, Iran 
; 
'Rasoul Vafazadeh ' 
; 
Department of Chemistry, 
Yazd University, 
Yazd, Iran 
; 
' Anthony C. Willis ' 
; 
Research School of Chemistry, 
The Australian National University, 
Canberra, A. C. T. 2601, Australia 
; 
#==============================================================================
# 4. TEXT                                                                     
_publ_section_abstract  #Text of the abstract                                 
;                                                                             
The crystal structure of 
[Ni(C~12~H~14~N~2~O~2~)~2~(CH~3~OH)~2~]Cl~2~
 is reported. 
;                                                                             
_publ_section_comment  #Text of the paper                                     
;                                                                             
The crystallographic asymmetric unit consists of 
one half of a 
[Ni(C~12~H~14~N~2~O~2~)~2~(CH~3~OH)~2~]^2+^ cation
and a chloride anion.
The other half of the cation is generated by
a crystallographic inversion symmetry operation.


;                                                                            
_publ_section_acknowledgements  # Acknowledgments                            
;                                                                            
; 
_publ_section_figure_captions  #Captions to figures                          
;                                                                            
?                                                                            
;                                                                            
_publ_section_exptl_refinement                                               
# see also _refine_ls_hydrogen for refinement keywords.                      
 
; 


;                                                                            
_publ_section_exptl_prep                                                     
;                                                                            
    The compound was prepared by ZM 
and recrystallised from methanol.
The sample identification was M3.
;                                                                            
 
 
_refine_special_details  #Text of the paper                                 
;                                                                            

The H atoms 
were all located in a difference electron density map, but 
those bonded to C 
 were repositioned geometrically. 
The H atoms were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98\%A, O---H = 0.83\%A) and with
U~iso~(H) in the range 1.2-1.5 times U~eq~ of the parent atom, 
after which the positions were refined without restraints.

The largest peaks in the final difference electron density map 
are located midway between bonded atoms or midway between H
atoms of methyl groups.

;                                                                            
 
 
 
# Insert your own references if required - in alphabetical order  
_publ_section_references  
;  


Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)

Spek, A.L. (2008). PLATON, A Multipurpose Crystallographic Tool, 
Utrecht University, 
Utrecht, The Netherlands.
 

; 


# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.5000 0.5000 0.5000 0.0160 1.0000 Uani S . . . . . 
Cl1 Cl 0.08551(5) 0.46249(2) 0.348455(17) 0.0276 1.0000 Uani . . . . . . 
O1 O 0.43351(15) 0.59720(5) 0.46876(5) 0.0208 1.0000 Uani . . . . . . 
O2 O 0.13581(15) 0.67273(6) 0.63177(6) 0.0245 1.0000 Uani . . . . . . 
O3 O 0.23118(15) 0.47176(6) 0.48486(5) 0.0247 1.0000 Uani . . . . . . 
N1 N 0.42520(16) 0.54580(6) 0.58756(6) 0.0165 1.0000 Uani . . . . . . 
N2 N 0.37981(17) 0.61573(6) 0.57581(6) 0.0186 1.0000 Uani . . . . . . 
C1 C 0.40925(19) 0.53311(7) 0.64889(7) 0.0174 1.0000 Uani . . . . . . 
C2 C 0.3506(2) 0.59437(7) 0.68805(7) 0.0206 1.0000 Uani . . . . . . 
C3 C 0.3182(2) 0.65271(7) 0.63751(7) 0.0190 1.0000 Uani . . . . . . 
C4 C 0.3829(2) 0.63724(7) 0.51324(7) 0.0188 1.0000 Uani . . . . . . 
C5 C 0.3243(3) 0.70947(8) 0.49720(8) 0.0272 1.0000 Uani . . . . . . 
C6 C 0.4487(3) 0.46428(8) 0.67764(8) 0.0248 1.0000 Uani . . . . . . 
C7 C 0.4382(2) 0.71565(8) 0.65051(6) 0.0194 1.0000 Uani . . . . . . 
C8 C 0.6269(2) 0.70583(9) 0.65793(7) 0.0250 1.0000 Uani . . . . . . 
C9 C 0.7389(2) 0.76123(10) 0.67333(8) 0.0316 1.0000 Uani . . . . . . 
C10 C 0.6652(3) 0.82725(9) 0.68021(8) 0.0331 1.0000 Uani . . . . . . 
C11 C 0.4796(3) 0.83734(9) 0.67229(8) 0.0307 1.0000 Uani . . . . . . 
C12 C 0.3648(2) 0.78166(8) 0.65812(7) 0.0244 1.0000 Uani . . . . . . 
C13 C 0.1387(3) 0.41762(10) 0.51877(10) 0.0335 1.0000 Uani . . . . . . 
H2 H 0.076(3) 0.6401(12) 0.6351(11) 0.0374 1.0000 Uiso . . . . . . 
H3 H 0.198(3) 0.4716(11) 0.4461(12) 0.0379 1.0000 Uiso . . . . . . 
H21 H 0.443(3) 0.6070(10) 0.7199(9) 0.0262 1.0000 Uiso . . . . . . 
H22 H 0.242(3) 0.5853(9) 0.7128(9) 0.0260 1.0000 Uiso . . . . . . 
H51 H 0.284(3) 0.7345(12) 0.5339(11) 0.0436 1.0000 Uiso . . . . . . 
H52 H 0.412(3) 0.7300(12) 0.4703(11) 0.0438 1.0000 Uiso . . . . . . 
H53 H 0.221(3) 0.7044(11) 0.4690(11) 0.0432 1.0000 Uiso . . . . . . 
H61 H 0.478(3) 0.4311(11) 0.6433(11) 0.0368 1.0000 Uiso . . . . . . 
H62 H 0.548(3) 0.4683(11) 0.7064(11) 0.0385 1.0000 Uiso . . . . . . 
H63 H 0.346(3) 0.4489(11) 0.7063(11) 0.0397 1.0000 Uiso . . . . . . 
H81 H 0.677(3) 0.6596(10) 0.6499(9) 0.0294 1.0000 Uiso . . . . . . 
H91 H 0.864(3) 0.7537(11) 0.6785(10) 0.0380 1.0000 Uiso . . . . . . 
H101 H 0.741(3) 0.8662(11) 0.6905(10) 0.0410 1.0000 Uiso . . . . . . 
H111 H 0.427(3) 0.8800(12) 0.6763(10) 0.0367 1.0000 Uiso . . . . . . 
H121 H 0.237(3) 0.7892(10) 0.6537(9) 0.0283 1.0000 Uiso . . . . . . 
H131 H 0.011(4) 0.4178(13) 0.5123(12) 0.0517 1.0000 Uiso . . . . . . 
H132 H 0.173(4) 0.3756(14) 0.5037(12) 0.0519 1.0000 Uiso . . . . . . 
H133 H 0.169(3) 0.4170(13) 0.5603(13) 0.0539 1.0000 Uiso . . . . . . 

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.02053(19) 0.01514(18) 0.01235(17) -0.00106(12) -0.00075(12) 0.00140(13) 
Cl1 0.0315(2) 0.0322(2) 0.01907(19) -0.00203(14) -0.00307(14) -0.00563(15) 
O1 0.0294(6) 0.0184(5) 0.0144(5) 0.0000(4) -0.0007(4) 0.0025(4) 
O2 0.0188(5) 0.0236(5) 0.0310(6) -0.0026(5) -0.0016(4) 0.0024(4) 
O3 0.0242(6) 0.0319(6) 0.0181(5) 0.0023(4) -0.0032(4) -0.0054(4) 
N1 0.0187(6) 0.0146(5) 0.0163(5) 0.0002(4) -0.0016(4) 0.0016(4) 
N2 0.0268(6) 0.0144(5) 0.0148(6) -0.0015(4) -0.0015(5) 0.0040(5) 
C1 0.0165(7) 0.0200(7) 0.0157(7) -0.0006(5) -0.0003(5) -0.0006(5) 
C2 0.0249(7) 0.0210(7) 0.0158(6) -0.0010(5) 0.0004(6) 0.0018(6) 
C3 0.0211(7) 0.0205(7) 0.0154(6) -0.0034(5) -0.0001(5) 0.0035(5) 
C4 0.0215(7) 0.0188(7) 0.0162(6) -0.0003(5) -0.0034(5) 0.0005(5) 
C5 0.0409(10) 0.0192(7) 0.0216(7) 0.0019(6) -0.0026(7) 0.0064(7) 
C6 0.0354(9) 0.0211(7) 0.0179(7) 0.0029(6) 0.0013(7) 0.0027(6) 
C7 0.0240(7) 0.0211(7) 0.0131(6) -0.0030(5) 0.0004(5) 0.0010(6) 
C8 0.0246(8) 0.0285(8) 0.0219(7) -0.0037(6) 0.0012(6) 0.0026(6) 
C9 0.0239(8) 0.0433(10) 0.0276(8) -0.0051(7) 0.0015(6) -0.0053(7) 
C10 0.0404(10) 0.0335(9) 0.0255(8) -0.0065(7) 0.0034(7) -0.0145(8) 
C11 0.0451(10) 0.0208(8) 0.0262(8) -0.0041(6) 0.0006(7) 0.0004(7) 
C12 0.0284(8) 0.0232(7) 0.0216(7) -0.0038(6) -0.0014(6) 0.0030(6) 
C13 0.0279(9) 0.0369(9) 0.0357(9) 0.0079(8) 0.0013(7) -0.0070(7) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 1.760(9) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Ni1 . O1 . 2.0372(10)    yes
Ni1 . O3 . 2.0606(11)    yes
Ni1 . N1 . 2.0674(12)    yes
O1 . C4 . 1.2476(18)    yes
O2 . C3 . 1.3914(18)    yes
O2 . H2 . 0.77(2)    no
O3 . C13 . 1.423(2)    yes
O3 . H3 . 0.83(2)    no
N1 . N2 . 1.4082(16)    yes
N1 . C1 . 1.2814(18)    yes
N2 . C3 . 1.5160(17)    yes
N2 . C4 . 1.3434(18)    yes
C1 . C2 . 1.4888(19)    yes
C1 . C6 . 1.479(2)    yes
C2 . C3 . 1.544(2)    yes
C2 . H21 . 0.97(2)    no
C2 . H22 . 0.96(2)    no
C3 . C7 . 1.520(2)    yes
C4 . C5 . 1.493(2)    yes
C5 . H51 . 0.94(2)    no
C5 . H52 . 0.93(2)    no
C5 . H53 . 0.95(2)    no
C6 . H61 . 0.97(2)    no
C6 . H62 . 0.94(2)    no
C6 . H63 . 0.99(2)    no
C7 . C8 . 1.399(2)    yes
C7 . C12 . 1.389(2)    yes
C8 . C9 . 1.381(2)    yes
C8 . H81 . 0.98(2)    no
C9 . C10 . 1.388(3)    yes
C9 . H91 . 0.93(2)    no
C10 . C11 . 1.379(3)    yes
C10 . H101 . 0.95(2)    no
C11 . C12 . 1.392(2)    yes
C11 . H111 . 0.91(2)    no
C12 . H121 . 0.95(2)    no
C13 . H131 . 0.94(3)    no
C13 . H132 . 0.90(3)    no
C13 . H133 . 0.88(3)    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
N1 2_666 Ni1 . O1 . 100.63(4)    yes
O3 2_666 Ni1 . O1 . 91.80(4)    yes
O1 2_666 Ni1 . O1 . 180.0    yes
N1 2_666 Ni1 . O3 . 90.53(5)    yes
O3 2_666 Ni1 . O3 . 180.0    yes
O1 . Ni1 . O3 . 88.20(4)    yes
N1 2_666 Ni1 . N1 . 180.0    yes
O1 . Ni1 . N1 . 79.37(4)    yes
O3 . Ni1 . N1 . 89.47(5)    yes
Ni1 . O1 . C4 . 114.27(9)    yes
C3 . O2 . H2 . 107.9(17)    no
Ni1 . O3 . C13 . 124.96(11)    yes
Ni1 . O3 . H3 . 114.8(16)    no
C13 . O3 . H3 . 109.1(15)    no
Ni1 . N1 . N2 . 108.86(8)    yes
Ni1 . N1 . C1 . 142.00(10)    yes
N2 . N1 . C1 . 109.12(11)    yes
N1 . N2 . C3 . 112.21(10)    yes
N1 . N2 . C4 . 116.95(11)    yes
C3 . N2 . C4 . 130.58(12)    yes
N1 . C1 . C2 . 113.58(12)    yes
N1 . C1 . C6 . 122.78(13)    yes
C2 . C1 . C6 . 123.63(12)    yes
C1 . C2 . C3 . 105.20(11)    yes
C1 . C2 . H21 . 111.0(11)    no
C3 . C2 . H21 . 111.9(11)    no
C1 . C2 . H22 . 112.1(11)    no
C3 . C2 . H22 . 111.1(11)    no
H21 . C2 . H22 . 105.8(15)    no
C2 . C3 . N2 . 99.66(11)    yes
C2 . C3 . O2 . 113.88(12)    yes
N2 . C3 . O2 . 110.16(11)    yes
C2 . C3 . C7 . 112.07(12)    yes
N2 . C3 . C7 . 110.43(11)    yes
O2 . C3 . C7 . 110.21(12)    yes
N2 . C4 . O1 . 120.44(13)    yes
N2 . C4 . C5 . 119.44(13)    yes
O1 . C4 . C5 . 120.12(13)    yes
C4 . C5 . H51 . 113.2(13)    no
C4 . C5 . H52 . 109.3(14)    no
H51 . C5 . H52 . 117.9(19)    no
C4 . C5 . H53 . 105.2(13)    no
H51 . C5 . H53 . 106.8(19)    no
H52 . C5 . H53 . 103.1(19)    no
C1 . C6 . H61 . 110.2(13)    no
C1 . C6 . H62 . 109.0(13)    no
H61 . C6 . H62 . 109.5(18)    no
C1 . C6 . H63 . 110.8(12)    no
H61 . C6 . H63 . 113.4(17)    no
H62 . C6 . H63 . 103.7(17)    no
C3 . C7 . C8 . 118.62(13)    yes
C3 . C7 . C12 . 121.85(14)    yes
C8 . C7 . C12 . 119.47(15)    yes
C7 . C8 . C9 . 120.23(15)    yes
C7 . C8 . H81 . 118.5(12)    no
C9 . C8 . H81 . 121.3(12)    no
C8 . C9 . C10 . 120.12(16)    yes
C8 . C9 . H91 . 119.1(14)    no
C10 . C9 . H91 . 120.8(14)    no
C9 . C10 . C11 . 119.88(16)    yes
C9 . C10 . H101 . 121.3(13)    no
C11 . C10 . H101 . 118.9(13)    no
C10 . C11 . C12 . 120.53(16)    yes
C10 . C11 . H111 . 122.1(14)    no
C12 . C11 . H111 . 117.4(14)    no
C11 . C12 . C7 . 119.76(16)    yes
C11 . C12 . H121 . 119.7(11)    no
C7 . C12 . H121 . 120.6(11)    no
O3 . C13 . H131 . 113.5(16)    no
O3 . C13 . H132 . 111.1(16)    no
H131 . C13 . H132 . 103(2)    no
O3 . C13 . H133 . 111.1(16)    no
H131 . C13 . H133 . 113(2)    no
H132 . C13 . H133 . 104(2)    no


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
 O3      Ni1     O1      C4        90.20(10)     .       .       .       .   no
 N1      Ni1     O1      C4         0.40(10)     .       .       .       .   no
 O3      Ni1     O1      C4       -89.80(10)   2_666     .       .       .   no
 N1      Ni1     O1      C4      -179.60(10)   2_666     .       .       .   no
 O1      Ni1     O3      C13     -153.21(13)     .       .       .       .   no
 N1      Ni1     O3      C13      -73.84(13)     .       .       .       .   no
 O1      Ni1     O3      C13       26.79(13)   2_666     .       .       .   no
 N1      Ni1     O3      C13      106.16(13)   2_666     .       .       .   no
 O1      Ni1     N1      N2         -2.08(8)     .       .       .       .   no
 O1      Ni1     N1      C1       179.85(17)     .       .       .       .   no
 O3      Ni1     N1      N2        -90.35(9)     .       .       .       .   no
 O3      Ni1     N1      C1        91.58(16)     .       .       .       .   no
 O1      Ni1     N1      N2        177.92(8)   2_666     .       .       .   no
 O1      Ni1     N1      C1        -0.15(17)   2_666     .       .       .   no
 O3      Ni1     N1      N2         89.65(9)   2_666     .       .       .   no
 O3      Ni1     N1      C1       -88.42(16)   2_666     .       .       .   no
 Ni1     O1      C4      N2         1.62(18)     .       .       .       .   no
 Ni1     O1      C4      C5      -178.07(12)     .       .       .       .   no
 Ni1     N1      N2      C3        178.45(9)     .       .       .       .   no
 Ni1     N1      N2      C4         3.61(14)     .       .       .       .   no
 C1      N1      N2      C3        -2.81(15)     .       .       .       .   no
 C1      N1      N2      C4      -177.65(13)     .       .       .       .   no
 Ni1     N1      C1      C2       177.68(11)     .       .       .       .   no
 Ni1     N1      C1      C6          -1.4(3)     .       .       .       .   no
 N2      N1      C1      C2        -0.39(16)     .       .       .       .   no
 N2      N1      C1      C6      -179.42(14)     .       .       .       .   no
 N1      N2      C3      O2      -115.54(12)     .       .       .       .   no
 N1      N2      C3      C2         4.45(14)     .       .       .       .   no
 N1      N2      C3      C7       122.50(12)     .       .       .       .   no
 C4      N2      C3      O2        58.40(19)     .       .       .       .   no
 C4      N2      C3      C2       178.39(14)     .       .       .       .   no
 C4      N2      C3      C7       -63.56(19)     .       .       .       .   no
 N1      N2      C4      O1          -3.7(2)     .       .       .       .   no
 N1      N2      C4      C5       176.02(14)     .       .       .       .   no
 C3      N2      C4      O1      -177.38(13)     .       .       .       .   no
 C3      N2      C4      C5           2.3(2)     .       .       .       .   no
 N1      C1      C2      C3         3.25(16)     .       .       .       .   no
 C6      C1      C2      C3      -177.72(15)     .       .       .       .   no
 C1      C2      C3      O2       112.93(13)     .       .       .       .   no
 C1      C2      C3      N2        -4.29(13)     .       .       .       .   no
 C1      C2      C3      C7      -121.12(12)     .       .       .       .   no
 O2      C3      C7      C8       179.85(12)     .       .       .       .   no
 O2      C3      C7      C12        2.83(18)     .       .       .       .   no
 N2      C3      C7      C8       -58.23(16)     .       .       .       .   no
 N2      C3      C7      C12      124.75(13)     .       .       .       .   no
 C2      C3      C7      C8        51.92(16)     .       .       .       .   no
 C2      C3      C7      C12     -125.10(14)     .       .       .       .   no
 C3      C7      C8      C9      -176.46(13)     .       .       .       .   no
 C12     C7      C8      C9           0.6(2)     .       .       .       .   no
 C3      C7      C12     C11      177.70(13)     .       .       .       .   no
 C8      C7      C12     C11          0.7(2)     .       .       .       .   no
 C7      C8      C9      C10         -1.3(2)     .       .       .       .   no
 C8      C9      C10     C11          0.7(2)     .       .       .       .   no
 C9      C10     C11     C12          0.7(2)     .       .       .       .   no
 C10     C11     C12     C7          -1.4(2)     .       .       .       .   no
 
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cl1     O3       2.9872(11)                     .       .                   no
 Cl1     O2       3.0925(12)                     .     2_566                 no
 Cl1     C1       3.6148(14)                     .     2_566                 no
 Cl1     C2       3.4855(15)                     .     7_564                 no
 Cl1     C13        3.605(2)                     .       .                   no
 Cl1     C2       3.4497(15)                     .     2_566                 no
O1      N1       2.6212(16)                     .       .                   no
 O1      N2       2.2496(16)                     .       .                   no
 O1      O3       2.8519(15)                     .       .                   no
 O1      C13        3.148(2)                     .     2_666                 no
 O1      O3       2.9427(15)                     .     2_666                 no
 O1      N1       3.1590(15)                     .     2_666                 no
 O1      C6         3.329(2)                     .     2_666                 no
O2      C5         3.154(2)                     .       .                   no
 O3      N1       2.9325(16)                     .     2_666                 no
 O3      N1       2.9055(16)                     .       .                   no
N1      C4       2.3459(18)                     .       .                   no
C5      C7         3.242(2)                     .       .                   no
 C5      C9         3.583(2)                     .     4_466                 no
C9      C12        3.585(2)                     .     8_556                 no

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
#
#D   H   A   D - H  H...A   D...A    D - H...A  symm(A)
#
O2      H2      Cl1        0.77(2)    2.33(2) 3.0925(12)  174.9(19)   2_566 yes
O3      H3      Cl1        0.83(2)    2.16(2) 2.9872(11)     173(2)     .   yes






_iucr_refine_instruction_details_constraints
;
#
# Punched on 22/06/15 at 16:40:17
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT NI   (    1 ,X'S,U'S)  UNTIL C    (   13 ) 
CONT H    (    2 ,X'S)  UNTIL H    (  133 ) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 22/06/15 at 16:40:17
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


#===END