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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_r2619
_database_code_depnum_ccdc_archive 'CCDC 1034090'
_audit_update_record             
;
2014-11-13 deposited with the CCDC.
2014-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Co2(LClO-tmpa)(Cl2(MeOH/H2O)2]PF6'
_chemical_formula_moiety         
'C34 H38 Cl3 Co2 N6 O3, C32 H34 Cl3 Co2 N6 O3, 2(F6 P)'
_chemical_formula_sum            'C66 H72 Cl6 Co4 F12 N12 O6 P2'
_chemical_formula_weight         1867.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Co Co 0.3494 0.9721 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   10.7772(10)
_cell_length_b                   11.8843(11)
_cell_length_c                   32.324(3)
_cell_angle_alpha                97.470(6)
_cell_angle_beta                 94.477(6)
_cell_angle_gamma                106.833(5)
_cell_volume                     3899.7(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4000
_cell_measurement_theta_min      2.00
_cell_measurement_theta_max      25.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1896
_exptl_absorpt_coefficient_mu    1.168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6991
_exptl_absorpt_correction_T_max  0.7915
_exptl_absorpt_process_details   SADABS

_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       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23532
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         0.64
_diffrn_reflns_theta_max         25.50
_reflns_number_total             23532
_reflns_number_gt                17766
_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    ?
_computing_publication_material  ?

_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)+(0.0973P)²+24.9940P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         23532
_refine_ls_number_parameters     994
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0705
_refine_ls_wR_factor_ref         0.2168
_refine_ls_wR_factor_gt          0.1821
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.004
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.64837(8) 1.05769(7) 0.59272(2) 0.0177(2) Uani 1 d . . .
Co2 Co 0.75544(8) 0.77823(7) 0.55777(2) 0.0185(2) Uani 1 d . . .
Cl3 Cl 0.70041(15) 1.10497(14) 0.52398(4) 0.0219(3) Uani 1 d . . .
Cl4 Cl 0.53250(16) 0.68507(14) 0.53147(5) 0.0265(4) Uani 1 d . . .
Cl1 Cl 1.07320(17) 1.02422(17) 0.76110(5) 0.0350(4) Uani 1 d . . .
Co3 Co 0.28450(8) 0.27273(7) 0.06515(2) 0.0182(2) Uani 1 d . . .
Co4 Co 0.61687(8) 0.22452(7) 0.10226(2) 0.0174(2) Uani 1 d . . .
Cl5 Cl 0.20738(16) 0.06320(14) 0.04222(5) 0.0289(4) Uani 1 d . . .
Cl6 Cl 0.67753(16) 0.27115(15) 0.03508(5) 0.0261(4) Uani 1 d . . .
N10 N 0.6061(5) 0.1863(4) 0.16592(15) 0.0171(11) Uani 1 d . . .
O2 O 0.4571(4) 0.2962(4) 0.10583(12) 0.0170(9) Uani 1 d . . .
P1 P 0.28586(16) 0.66841(15) 0.67096(5) 0.0202(4) Uani 1 d . . .
P2 P 0.24208(18) 0.82757(16) 0.17367(5) 0.0264(4) Uani 1 d . . .
F5 F 0.1598(3) 0.6035(3) 0.63741(11) 0.0266(9) Uani 1 d . . .
F6 F 0.4107(4) 0.7336(4) 0.70473(13) 0.0409(11) Uani 1 d . . .
F8 F 0.3689(4) 0.7986(4) 0.15883(16) 0.0503(12) Uani 1 d . . .
F9 F 0.2612(5) 0.9264(4) 0.14458(17) 0.0585(14) Uani 1 d . . .
F4 F 0.2529(5) 0.7901(4) 0.67264(15) 0.0499(12) Uani 1 d . . .
F1 F 0.1959(5) 0.6362(5) 0.70735(13) 0.0615(15) Uani 1 d . . .
F3 F 0.3701(4) 0.7024(5) 0.63410(14) 0.0605(15) Uani 1 d . . .
F11 F 0.1530(4) 0.7294(4) 0.13630(14) 0.0485(12) Uani 1 d . . .
F12 F 0.3331(5) 0.9237(5) 0.21105(14) 0.0659(16) Uani 1 d . . .
F10 F 0.1151(5) 0.8530(5) 0.1880(2) 0.092(2) Uani 1 d . . .
F7 F 0.2250(6) 0.7264(5) 0.20198(17) 0.086(2) Uani 1 d . . .
F2 F 0.3172(5) 0.5462(4) 0.6694(2) 0.081(2) Uani 1 d . . .
Cl2 Cl 0.5044(2) 0.61333(16) 0.26586(5) 0.0359(4) Uani 1 d . . .
O1 O 0.7457(4) 0.9310(4) 0.59830(12) 0.0207(10) Uani 1 d . . .
N3 N 0.8099(5) 1.1953(5) 0.62749(15) 0.0192(11) Uani 1 d . . .
N1 N 0.5979(5) 1.0537(5) 0.65684(15) 0.0189(11) Uani 1 d . . .
N2 N 0.5150(5) 1.1629(5) 0.59700(16) 0.0264(13) Uani 1 d . . .
N6 N 0.7572(5) 0.6890(5) 0.60913(16) 0.0200(12) Uani 1 d . . .
N4 N 0.9645(5) 0.8289(4) 0.57644(15) 0.0183(11) Uani 1 d . . .
N5 N 0.8244(5) 0.6613(5) 0.51388(15) 0.0208(12) Uani 1 d . . .
N12 N 0.7471(5) 0.3847(5) 0.13635(15) 0.0199(12) Uani 1 d . . .
N11 N 0.7374(5) 0.1079(5) 0.10766(16) 0.0231(12) Uani 1 d . . .
N8 N 0.1821(5) 0.2730(5) 0.11798(16) 0.0224(12) Uani 1 d . . .
N7 N 0.3077(5) 0.4612(4) 0.07991(15) 0.0199(12) Uani 1 d . . .
N9 N 0.1432(5) 0.3016(4) 0.01905(15) 0.0180(11) Uani 1 d . . .
C3 C 0.8425(6) 0.9792(6) 0.71226(19) 0.0237(15) Uani 1 d . . .
H3 H 0.8050 0.9830 0.7378 0.028 Uiso 1 calc R . .
C6 C 0.9544(6) 0.9684(5) 0.63779(18) 0.0178(13) Uani 1 d . . .
C2 C 0.7628(6) 0.9576(5) 0.67383(18) 0.0171(13) Uani 1 d . . .
C4 C 0.9740(6) 0.9951(6) 0.71336(18) 0.0220(14) Uani 1 d . . .
C1 C 0.8196(6) 0.9506(5) 0.63601(18) 0.0158(13) Uani 1 d . . .
C5 C 1.0310(6) 0.9903(5) 0.67644(18) 0.0204(14) Uani 1 d . . .
H5 H 1.1223 1.0021 0.6775 0.024 Uiso 1 calc R . .
C7 C 0.6207(6) 0.9482(6) 0.67221(19) 0.0215(14) Uani 1 d . . .
H7A H 0.5682 0.8748 0.6532 0.026 Uiso 1 calc R . .
H7B H 0.5931 0.9435 0.7006 0.026 Uiso 1 calc R . .
C10 C 0.3618(7) 1.2159(7) 0.6393(2) 0.0342(18) Uani 1 d . . .
H10 H 0.3085 1.2015 0.6612 0.041 Uiso 1 calc R . .
C15 C 0.8066(6) 1.2192(5) 0.66924(19) 0.0212(14) Uani 1 d . . .
C14 C 0.6779(6) 1.1662(5) 0.68460(19) 0.0204(14) Uani 1 d . . .
H14A H 0.6937 1.1494 0.7134 0.024 Uiso 1 calc R . .
H14B H 0.6285 1.2247 0.6859 0.024 Uiso 1 calc R . .
C19 C 0.9217(6) 1.2451(6) 0.61260(19) 0.0227(15) Uani 1 d . . .
H19 H 0.9267 1.2252 0.5835 0.027 Uiso 1 calc R . .
C9 C 0.4419(6) 1.1444(6) 0.62895(19) 0.0247(15) Uani 1 d . . .
C16 C 0.9134(7) 1.2943(6) 0.6960(2) 0.0312(17) Uani 1 d . . .
H16 H 0.9083 1.3097 0.7253 0.037 Uiso 1 calc R . .
C13 C 0.5114(7) 1.2483(6) 0.5755(2) 0.0313(17) Uani 1 d . . .
H13 H 0.5620 1.2587 0.5527 0.038 Uiso 1 calc R . .
C18 C 1.0279(7) 1.3220(6) 0.6367(2) 0.0317(17) Uani 1 d . . .
H18 H 1.1031 1.3594 0.6243 0.038 Uiso 1 calc R . .
C17 C 1.0259(7) 1.3461(7) 0.6800(2) 0.0359(19) Uani 1 d . . .
H17 H 1.1006 1.3970 0.6979 0.043 Uiso 1 calc R . .
C11 C 0.3616(8) 1.3073(7) 0.6170(3) 0.046(2) Uani 1 d . . .
H11 H 0.3099 1.3579 0.6241 0.056 Uiso 1 calc R . .
C8 C 0.4574(6) 1.0480(6) 0.6529(2) 0.0269(15) Uani 1 d . . .
H8A H 0.4291 1.0599 0.6811 0.032 Uiso 1 calc R . .
H8B H 0.4031 0.9691 0.6377 0.032 Uiso 1 calc R . .
C12 C 0.4372(8) 1.3246(7) 0.5844(2) 0.043(2) Uani 1 d . . .
H12 H 0.4384 1.3868 0.5686 0.051 Uiso 1 calc R . .
C25 C 0.8022(7) 0.4985(6) 0.45865(18) 0.0234(15) Uani 1 d . . .
H25 H 0.7477 0.4286 0.4410 0.028 Uiso 1 calc R . .
C22 C 0.9514(7) 0.7017(6) 0.50981(18) 0.0226(15) Uani 1 d . . .
C20 C 1.0148(6) 0.9562(5) 0.59826(18) 0.0199(14) Uani 1 d . . .
H20A H 1.1110 0.9800 0.6048 0.024 Uiso 1 calc R . .
H20B H 0.9928 1.0093 0.5796 0.024 Uiso 1 calc R . .
C21 C 1.0268(6) 0.8161(6) 0.53735(19) 0.0230(15) Uani 1 d . . .
H21A H 1.1180 0.8166 0.5445 0.028 Uiso 1 calc R . .
H21B H 1.0284 0.8838 0.5223 0.028 Uiso 1 calc R . .
C24 C 0.9307(7) 0.5413(6) 0.45428(18) 0.0258(16) Uani 1 d . . .
H24 H 0.9673 0.5013 0.4334 0.031 Uiso 1 calc R . .
C23 C 1.0092(7) 0.6442(6) 0.48047(18) 0.0226(14) Uani 1 d . . .
H23 H 1.0998 0.6742 0.4783 0.027 Uiso 1 calc R . .
C26 C 0.7517(7) 0.5599(6) 0.48985(19) 0.0231(14) Uani 1 d . . .
H26 H 0.6628 0.5283 0.4940 0.028 Uiso 1 calc R . .
C32 C 0.6506(7) 0.6395(6) 0.6278(2) 0.0250(15) Uani 1 d . . .
H32 H 0.5667 0.6347 0.6148 0.030 Uiso 1 calc R . .
C27 C 0.9897(6) 0.7470(6) 0.6043(2) 0.0228(14) Uani 1 d . . .
H27A H 1.0670 0.7902 0.6250 0.027 Uiso 1 calc R . .
H27B H 1.0104 0.6808 0.5873 0.027 Uiso 1 calc R . .
C29 C 0.8910(7) 0.6534(7) 0.6653(2) 0.0322(17) Uani 1 d . . .
H29 H 0.9756 0.6592 0.6780 0.039 Uiso 1 calc R . .
C28 C 0.8754(6) 0.6959(5) 0.62764(19) 0.0216(14) Uani 1 d . . .
C31 C 0.6598(7) 0.5965(6) 0.6646(2) 0.0289(16) Uani 1 d . . .
H31 H 0.5835 0.5623 0.6770 0.035 Uiso 1 calc R . .
C30 C 0.7819(7) 0.6030(7) 0.6837(2) 0.0381(19) Uani 1 d . . .
H30 H 0.7901 0.5729 0.7093 0.046 Uiso 1 calc R . .
C51 C 0.0431(6) 0.2191(5) -0.00531(18) 0.0198(14) Uani 1 d . . .
H51 H 0.0202 0.1398 0.0005 0.024 Uiso 1 calc R . .
C50 C -0.0280(7) 0.2437(6) -0.03834(19) 0.0227(14) Uani 1 d . . .
H50 H -0.0988 0.1833 -0.0548 0.027 Uiso 1 calc R . .
C33 C 0.4653(6) 0.3683(5) 0.14270(17) 0.0177(13) Uani 1 d . . .
C37 C 0.4899(6) 0.4033(6) 0.21922(19) 0.0218(14) Uani 1 d . . .
H37 H 0.4984 0.3756 0.2453 0.026 Uiso 1 calc R . .
C41 C 0.1694(6) 0.3802(6) 0.1337(2) 0.0258(15) Uani 1 d . . .
C38 C 0.4792(6) 0.3273(5) 0.18089(18) 0.0182(13) Uani 1 d . . .
C36 C 0.4878(6) 0.5178(6) 0.21829(19) 0.0233(15) Uani 1 d . . .
C34 C 0.4630(6) 0.4856(5) 0.14274(18) 0.0190(13) Uani 1 d . . .
C49 C 0.0069(6) 0.3580(6) -0.04661(19) 0.0224(14) Uani 1 d . . .
H49 H -0.0385 0.3771 -0.0698 0.027 Uiso 1 calc R . .
C40 C 0.2048(7) 0.4745(6) 0.1059(2) 0.0281(16) Uani 1 d . . .
H40A H 0.1258 0.4705 0.0872 0.034 Uiso 1 calc R . .
H40B H 0.2348 0.5539 0.1237 0.034 Uiso 1 calc R . .
C35 C 0.4735(6) 0.5603(6) 0.18102(18) 0.0223(14) Uani 1 d . . .
H35 H 0.4708 0.6396 0.1813 0.027 Uiso 1 calc R . .
C48 C 0.1070(6) 0.4454(6) -0.02166(18) 0.0197(14) Uani 1 d . . .
H48 H 0.1297 0.5253 -0.0268 0.024 Uiso 1 calc R . .
C39 C 0.4397(6) 0.5282(6) 0.10226(19) 0.0221(14) Uani 1 d . . .
H39A H 0.5069 0.5181 0.0841 0.027 Uiso 1 calc R . .
H39B H 0.4479 0.6141 0.1079 0.027 Uiso 1 calc R . .
C43 C 0.0910(7) 0.3062(9) 0.1948(2) 0.048(2) Uani 1 d . . .
H43 H 0.0601 0.3177 0.2213 0.057 Uiso 1 calc R . .
C42 C 0.1229(7) 0.3976(7) 0.1721(2) 0.0348(18) Uani 1 d . . .
H42 H 0.1133 0.4727 0.1825 0.042 Uiso 1 calc R . .
C47 C 0.1737(6) 0.4143(5) 0.01104(17) 0.0173(13) Uani 1 d . . .
C45 C 0.1519(6) 0.1829(7) 0.14037(19) 0.0263(16) Uani 1 d . . .
H45 H 0.1632 0.1086 0.1298 0.032 Uiso 1 calc R . .
C46 C 0.2879(7) 0.5031(6) 0.03898(19) 0.0275(16) Uani 1 d . . .
H46A H 0.3678 0.5133 0.0248 0.033 Uiso 1 calc R . .
H46B H 0.2715 0.5812 0.0441 0.033 Uiso 1 calc R . .
C44 C 0.1038(7) 0.1975(8) 0.1791(2) 0.043(2) Uani 1 d . . .
H44 H 0.0804 0.1329 0.1944 0.052 Uiso 1 calc R . .
C52 C 0.4842(6) 0.2011(6) 0.18144(18) 0.0194(14) Uani 1 d . . .
H52A H 0.4808 0.1831 0.2105 0.023 Uiso 1 calc R . .
H52B H 0.4074 0.1441 0.1634 0.023 Uiso 1 calc R . .
C58 C 0.8245(6) 0.0898(6) 0.0821(2) 0.0235(15) Uani 1 d . . .
H58 H 0.8451 0.1382 0.0609 0.028 Uiso 1 calc R . .
C64 C 0.7886(6) 0.4886(6) 0.1217(2) 0.0247(15) Uani 1 d . . .
H64 H 0.7706 0.4888 0.0925 0.030 Uiso 1 calc R . .
C63 C 0.8559(7) 0.5944(6) 0.1471(2) 0.0310(17) Uani 1 d . . .
H63 H 0.8856 0.6653 0.1354 0.037 Uiso 1 calc R . .
C62 C 0.8798(7) 0.5965(6) 0.1899(2) 0.0322(17) Uani 1 d . . .
H62 H 0.9259 0.6687 0.2080 0.039 Uiso 1 calc R . .
C54 C 0.7075(6) 0.0384(5) 0.1373(2) 0.0212(14) Uani 1 d . . .
C61 C 0.8357(7) 0.4920(6) 0.2059(2) 0.0300(17) Uani 1 d . . .
H61 H 0.8507 0.4908 0.2352 0.036 Uiso 1 calc R . .
C60 C 0.7685(6) 0.3879(6) 0.17827(18) 0.0189(14) Uani 1 d . . .
C53 C 0.6070(6) 0.0614(6) 0.1647(2) 0.0225(14) Uani 1 d . . .
H53A H 0.5195 0.0063 0.1532 0.027 Uiso 1 calc R . .
H53B H 0.6283 0.0470 0.1935 0.027 Uiso 1 calc R . .
C56 C 0.8546(7) -0.0687(7) 0.1157(2) 0.0336(18) Uani 1 d . . .
H56 H 0.8955 -0.1287 0.1185 0.040 Uiso 1 calc R . .
C57 C 0.8849(6) 0.0037(6) 0.0856(2) 0.0288(16) Uani 1 d . . .
H57 H 0.9472 -0.0059 0.0673 0.035 Uiso 1 calc R . .
C59 C 0.7244(6) 0.2679(6) 0.19273(18) 0.0215(14) Uani 1 d . . .
H59A H 0.7960 0.2312 0.1919 0.026 Uiso 1 calc R . .
H59B H 0.7054 0.2792 0.2222 0.026 Uiso 1 calc R . .
C55 C 0.7627(6) -0.0521(6) 0.1421(2) 0.0265(15) Uani 1 d . . .
H55 H 0.7384 -0.1015 0.1628 0.032 Uiso 1 calc R . .
O3 O 0.4768(4) 0.9158(4) 0.56485(13) 0.0243(10) Uani 1 d D . .
H91 H 0.4286(11) 0.9202(10) 0.5434(4) 0.032 Uiso 1 d D . .
H92 H 0.4983(11) 0.8544(10) 0.5592(4) 0.032 Uiso 1 d D . .
O6 O 0.4746(4) 0.0618(4) 0.07703(15) 0.0319(11) Uani 1 d D . .
H96 H 0.4027(10) 0.0745(9) 0.0718(4) 0.048 Uiso 1 d D . .
O4 O 0.7782(5) 0.8805(4) 0.50613(13) 0.0333(12) Uani 1 d D . .
H93 H 0.7552(11) 0.9416(9) 0.5122(4) 0.045 Uiso 1 d D . .
H94 H 0.7487(11) 0.8519(9) 0.4804(4) 0.045 Uiso 1 d D . .
O5 O 0.4107(4) 0.3057(4) 0.01657(13) 0.0296(11) Uani 1 d D . .
H95 H 0.4854(10) 0.2963(9) 0.0217(4) 0.045 Uiso 1 d D . .
C90 C 0.3754(12) 0.2569(12) -0.0258(3) 0.058(4) Uani 1 d . . .
H90A H 0.3459 0.1698 -0.0288 0.075 Uiso 1 calc R . .
H90B H 0.4510 0.2822 -0.0412 0.075 Uiso 1 calc R . .
H90C H 0.3046 0.2845 -0.0373 0.075 Uiso 1 calc R . .
C91 C 0.476(2) -0.0437(14) 0.0538(6) 0.097(7) Uani 1 d . . .
H91A H 0.5630 -0.0342 0.0448 0.126 Uiso 1 calc R . .
H91B H 0.4107 -0.0647 0.0290 0.126 Uiso 1 calc R . .
H91C H 0.4563 -0.1071 0.0711 0.126 Uiso 1 calc R . .


_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
Co1 O1 2.087(4) . ?
Co1 N3 2.130(5) . ?
Co1 O3 2.148(4) . ?
Co1 N2 2.162(6) . ?
Co1 N1 2.187(5) . ?
Co1 Cl3 2.4298(16) . ?
Co2 N6 2.085(5) . ?
Co2 O1 2.130(4) . ?
Co2 N4 2.171(5) . ?
Co2 N5 2.178(5) . ?
Co2 O4 2.178(5) . ?
Co2 Cl4 2.3700(18) . ?
Cl1 C4 1.742(6) . ?
Co3 N8 2.105(5) . ?
Co3 O2 2.119(4) . ?
Co3 O5 2.157(4) . ?
Co3 N7 2.165(5) . ?
Co3 N9 2.177(5) . ?
Co3 Cl5 2.3804(18) . ?
Co4 N12 2.116(5) . ?
Co4 O6 2.105(5) . ?
Co4 O2 2.135(4) . ?
Co4 N10 2.169(5) . ?
Co4 N11 2.170(5) . ?
Co4 Cl6 2.4030(17) . ?
N10 C53 1.483(8) . ?
N10 C59 1.487(8) . ?
N10 C52 1.490(8) . ?
O2 C33 1.355(7) . ?
P1 F3 1.578(5) . ?
P1 F2 1.579(5) . ?
P1 F4 1.582(4) . ?
P1 F6 1.596(4) . ?
P1 F1 1.597(5) . ?
P1 F5 1.601(4) . ?
P2 F10 1.575(5) . ?
P2 F9 1.576(5) . ?
P2 F7 1.581(5) . ?
P2 F12 1.592(4) . ?
P2 F11 1.595(4) . ?
P2 F8 1.596(5) . ?
Cl2 C36 1.753(6) . ?
O1 C1 1.357(7) . ?
N3 C19 1.336(8) . ?
N3 C15 1.348(8) . ?
N1 C7 1.483(8) . ?
N1 C8 1.490(8) . ?
N1 C14 1.496(8) . ?
N2 C13 1.311(9) . ?
N2 C9 1.350(9) . ?
N6 C28 1.340(8) . ?
N6 C32 1.357(8) . ?
N4 C27 1.474(8) . ?
N4 C21 1.487(7) . ?
N4 C20 1.507(8) . ?
N5 C26 1.335(8) . ?
N5 C22 1.337(8) . ?
N12 C60 1.350(8) . ?
N12 C64 1.347(8) . ?
N11 C54 1.344(8) . ?
N11 C58 1.342(8) . ?
N8 C45 1.346(8) . ?
N8 C41 1.357(9) . ?
N7 C40 1.474(8) . ?
N7 C39 1.488(8) . ?
N7 C46 1.494(8) . ?
N9 C51 1.341(8) . ?
N9 C47 1.348(8) . ?
C3 C4 1.371(9) . ?
C3 C2 1.403(8) . ?
C6 C5 1.393(8) . ?
C6 C1 1.401(9) . ?
C6 C20 1.487(8) . ?
C2 C1 1.413(8) . ?
C2 C7 1.499(9) . ?
C4 C5 1.386(9) . ?
C10 C11 1.378(11) . ?
C10 C9 1.405(9) . ?
C15 C16 1.384(9) . ?
C15 C14 1.500(9) . ?
C19 C18 1.350(9) . ?
C9 C8 1.503(10) . ?
C16 C17 1.365(10) . ?
C13 C12 1.390(10) . ?
C18 C17 1.395(9) . ?
C11 C12 1.382(12) . ?
C25 C24 1.355(10) . ?
C25 C26 1.404(9) . ?
C22 C23 1.386(9) . ?
C22 C21 1.494(9) . ?
C24 C23 1.396(9) . ?
C32 C31 1.361(9) . ?
C27 C28 1.511(9) . ?
C29 C30 1.375(10) . ?
C29 C28 1.395(9) . ?
C31 C30 1.386(10) . ?
C51 C50 1.377(9) . ?
C50 C49 1.369(9) . ?
C33 C38 1.398(8) . ?
C33 C34 1.401(9) . ?
C37 C36 1.371(9) . ?
C37 C38 1.411(8) . ?
C41 C42 1.387(9) . ?
C41 C40 1.508(10) . ?
C38 C52 1.519(9) . ?
C36 C35 1.380(9) . ?
C34 C35 1.403(8) . ?
C34 C39 1.492(8) . ?
C49 C48 1.375(9) . ?
C48 C47 1.381(8) . ?
C43 C42 1.367(11) . ?
C43 C44 1.375(13) . ?
C47 C46 1.506(9) . ?
C45 C44 1.401(10) . ?
C58 C57 1.374(9) . ?
C64 C63 1.376(9) . ?
C63 C62 1.383(10) . ?
C62 C61 1.377(10) . ?
C54 C55 1.390(9) . ?
C54 C53 1.514(9) . ?
C61 C60 1.394(9) . ?
C60 C59 1.515(9) . ?
C56 C55 1.396(10) . ?
C56 C57 1.380(10) . ?

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
O1 Co1 N3 91.38(18) . . ?
O1 Co1 O3 88.66(17) . . ?
N3 Co1 O3 173.04(18) . . ?
O1 Co1 N2 165.3(2) . . ?
N3 Co1 N2 94.4(2) . . ?
O3 Co1 N2 83.94(19) . . ?
O1 Co1 N1 91.28(17) . . ?
N3 Co1 N1 78.62(19) . . ?
O3 Co1 N1 94.42(18) . . ?
N2 Co1 N1 76.7(2) . . ?
O1 Co1 Cl3 99.76(12) . . ?
N3 Co1 Cl3 95.63(14) . . ?
O3 Co1 Cl3 91.21(12) . . ?
N2 Co1 Cl3 93.11(15) . . ?
N1 Co1 Cl3 167.72(15) . . ?
N6 Co2 O1 89.92(18) . . ?
N6 Co2 N4 80.4(2) . . ?
O1 Co2 N4 89.88(17) . . ?
N6 Co2 N5 97.87(19) . . ?
O1 Co2 N5 161.83(19) . . ?
N4 Co2 N5 75.39(19) . . ?
N6 Co2 O4 173.3(2) . . ?
O1 Co2 O4 89.37(16) . . ?
N4 Co2 O4 92.94(19) . . ?
N5 Co2 O4 80.97(18) . . ?
N6 Co2 Cl4 96.74(16) . . ?
O1 Co2 Cl4 101.58(13) . . ?
N4 Co2 Cl4 168.22(14) . . ?
N5 Co2 Cl4 93.81(15) . . ?
O4 Co2 Cl4 89.94(15) . . ?
N8 Co3 O2 88.93(17) . . ?
N8 Co3 O5 169.2(2) . . ?
O2 Co3 O5 85.83(16) . . ?
N8 Co3 N7 80.2(2) . . ?
O2 Co3 N7 90.05(17) . . ?
O5 Co3 N7 90.36(19) . . ?
N8 Co3 N9 99.44(19) . . ?
O2 Co3 N9 162.15(18) . . ?
O5 Co3 N9 83.19(17) . . ?
N7 Co3 N9 76.02(19) . . ?
N8 Co3 Cl5 96.31(16) . . ?
O2 Co3 Cl5 103.31(12) . . ?
O5 Co3 Cl5 94.03(14) . . ?
N7 Co3 Cl5 166.19(15) . . ?
N9 Co3 Cl5 91.49(14) . . ?
N12 Co4 O6 171.17(19) . . ?
N12 Co4 O2 91.01(18) . . ?
O6 Co4 O2 85.73(17) . . ?
N12 Co4 N10 79.59(19) . . ?
O6 Co4 N10 92.26(19) . . ?
O2 Co4 N10 91.12(17) . . ?
N12 Co4 N11 99.4(2) . . ?
O6 Co4 N11 81.71(19) . . ?
O2 Co4 N11 161.58(18) . . ?
N10 Co4 N11 76.04(19) . . ?
N12 Co4 Cl6 94.13(14) . . ?
O6 Co4 Cl6 94.50(15) . . ?
O2 Co4 Cl6 99.59(11) . . ?
N10 Co4 Cl6 167.73(14) . . ?
N11 Co4 Cl6 94.80(15) . . ?
C53 N10 C59 109.6(5) . . ?
C53 N10 C52 110.3(5) . . ?
C59 N10 C52 111.5(5) . . ?
C53 N10 Co4 106.9(4) . . ?
C59 N10 Co4 107.9(4) . . ?
C52 N10 Co4 110.6(3) . . ?
C33 O2 Co3 113.2(3) . . ?
C33 O2 Co4 113.1(3) . . ?
Co3 O2 Co4 133.65(19) . . ?
F3 P1 F2 91.5(4) . . ?
F3 P1 F4 89.0(3) . . ?
F2 P1 F4 179.4(3) . . ?
F3 P1 F6 90.4(2) . . ?
F2 P1 F6 91.1(3) . . ?
F4 P1 F6 89.3(2) . . ?
F3 P1 F1 177.5(3) . . ?
F2 P1 F1 90.3(4) . . ?
F4 P1 F1 89.1(3) . . ?
F6 P1 F1 91.2(2) . . ?
F3 P1 F5 90.1(2) . . ?
F2 P1 F5 89.2(2) . . ?
F4 P1 F5 90.4(2) . . ?
F6 P1 F5 179.4(2) . . ?
F1 P1 F5 88.3(2) . . ?
F10 P2 F9 91.3(4) . . ?
F10 P2 F7 90.2(4) . . ?
F9 P2 F7 178.3(4) . . ?
F10 P2 F12 92.1(3) . . ?
F9 P2 F12 89.7(3) . . ?
F7 P2 F12 91.0(3) . . ?
F10 P2 F11 89.0(3) . . ?
F9 P2 F11 91.0(3) . . ?
F7 P2 F11 88.2(3) . . ?
F12 P2 F11 178.7(3) . . ?
F10 P2 F8 178.7(3) . . ?
F9 P2 F8 89.5(3) . . ?
F7 P2 F8 89.0(3) . . ?
F12 P2 F8 88.9(3) . . ?
F11 P2 F8 90.0(3) . . ?
C1 O1 Co1 113.0(3) . . ?
C1 O1 Co2 112.9(3) . . ?
Co1 O1 Co2 134.2(2) . . ?
C19 N3 C15 117.5(5) . . ?
C19 N3 Co1 125.0(4) . . ?
C15 N3 Co1 116.6(4) . . ?
C7 N1 C8 112.7(5) . . ?
C7 N1 C14 110.9(5) . . ?
C8 N1 C14 110.0(5) . . ?
C7 N1 Co1 109.5(3) . . ?
C8 N1 Co1 103.9(4) . . ?
C14 N1 Co1 109.5(4) . . ?
C13 N2 C9 119.7(6) . . ?
C13 N2 Co1 126.4(5) . . ?
C9 N2 Co1 113.3(4) . . ?
C28 N6 C32 118.7(5) . . ?
C28 N6 Co2 115.9(4) . . ?
C32 N6 Co2 124.8(4) . . ?
C27 N4 C21 110.5(5) . . ?
C27 N4 C20 111.1(5) . . ?
C21 N4 C20 109.5(5) . . ?
C27 N4 Co2 108.0(4) . . ?
C21 N4 Co2 107.0(4) . . ?
C20 N4 Co2 110.6(4) . . ?
C26 N5 C22 118.8(5) . . ?
C26 N5 Co2 126.6(4) . . ?
C22 N5 Co2 114.5(4) . . ?
C60 N12 C64 117.3(5) . . ?
C60 N12 Co4 115.7(4) . . ?
C64 N12 Co4 125.7(4) . . ?
C54 N11 C58 118.6(6) . . ?
C54 N11 Co4 113.8(4) . . ?
C58 N11 Co4 127.1(5) . . ?
C45 N8 C41 119.6(6) . . ?
C45 N8 Co3 124.2(5) . . ?
C41 N8 Co3 115.0(4) . . ?
C40 N7 C39 111.0(5) . . ?
C40 N7 C46 110.0(5) . . ?
C39 N7 C46 110.3(5) . . ?
C40 N7 Co3 107.4(4) . . ?
C39 N7 Co3 111.4(4) . . ?
C46 N7 Co3 106.5(4) . . ?
C51 N9 C47 118.1(5) . . ?
C51 N9 Co3 127.5(4) . . ?
C47 N9 Co3 113.7(4) . . ?
C4 C3 C2 120.8(6) . . ?
C5 C6 C1 120.3(6) . . ?
C5 C6 C20 119.7(5) . . ?
C1 C6 C20 119.9(5) . . ?
C1 C2 C3 119.0(6) . . ?
C1 C2 C7 119.5(5) . . ?
C3 C2 C7 121.4(5) . . ?
C3 C4 C5 120.6(6) . . ?
C3 C4 Cl1 120.8(5) . . ?
C5 C4 Cl1 118.6(5) . . ?
O1 C1 C6 120.1(5) . . ?
O1 C1 C2 120.6(5) . . ?
C6 C1 C2 119.3(5) . . ?
C4 C5 C6 119.9(6) . . ?
N1 C7 C2 109.8(5) . . ?
C11 C10 C9 119.1(7) . . ?
N3 C15 C16 121.9(6) . . ?
N3 C15 C14 116.0(5) . . ?
C16 C15 C14 121.9(6) . . ?
N1 C14 C15 112.2(5) . . ?
N3 C19 C18 123.6(6) . . ?
N2 C9 C10 120.5(7) . . ?
N2 C9 C8 115.6(5) . . ?
C10 C9 C8 123.9(6) . . ?
C17 C16 C15 119.7(6) . . ?
N2 C13 C12 123.2(7) . . ?
C19 C18 C17 119.2(6) . . ?
C16 C17 C18 118.0(6) . . ?
C10 C11 C12 119.5(7) . . ?
N1 C8 C9 108.1(5) . . ?
C11 C12 C13 118.0(8) . . ?
C24 C25 C26 118.4(6) . . ?
N5 C22 C23 122.3(6) . . ?
N5 C22 C21 116.0(5) . . ?
C23 C22 C21 121.7(6) . . ?
C6 C20 N4 109.5(5) . . ?
N4 C21 C22 109.5(5) . . ?
C25 C24 C23 119.9(6) . . ?
C22 C23 C24 118.3(6) . . ?
N5 C26 C25 122.2(6) . . ?
N6 C32 C31 122.3(6) . . ?
N4 C27 C28 113.1(5) . . ?
C30 C29 C28 118.8(6) . . ?
N6 C28 C29 121.7(6) . . ?
N6 C28 C27 116.1(5) . . ?
C29 C28 C27 122.1(6) . . ?
C32 C31 C30 119.2(6) . . ?
C29 C30 C31 119.3(6) . . ?
N9 C51 C50 123.2(6) . . ?
C49 C50 C51 117.8(6) . . ?
O2 C33 C38 120.3(5) . . ?
O2 C33 C34 120.0(5) . . ?
C38 C33 C34 119.6(5) . . ?
C36 C37 C38 119.0(6) . . ?
N8 C41 C42 121.0(7) . . ?
N8 C41 C40 115.2(6) . . ?
C42 C41 C40 123.8(6) . . ?
C33 C38 C37 120.2(6) . . ?
C33 C38 C52 120.3(5) . . ?
C37 C38 C52 119.5(5) . . ?
C37 C36 C35 122.0(6) . . ?
C37 C36 Cl2 119.1(5) . . ?
C35 C36 Cl2 118.9(5) . . ?
C33 C34 C35 119.7(5) . . ?
C33 C34 C39 120.2(5) . . ?
C35 C34 C39 119.9(5) . . ?
C48 C49 C50 120.5(6) . . ?
N7 C40 C41 112.9(5) . . ?
C36 C35 C34 119.5(6) . . ?
C49 C48 C47 118.5(6) . . ?
C34 C39 N7 111.2(5) . . ?
C42 C43 C44 119.6(7) . . ?
C43 C42 C41 119.7(7) . . ?
N9 C47 C48 121.9(6) . . ?
N9 C47 C46 115.9(5) . . ?
C48 C47 C46 122.2(6) . . ?
N8 C45 C44 120.7(7) . . ?
N7 C46 C47 110.3(5) . . ?
C43 C44 C45 119.4(7) . . ?
N10 C52 C38 110.7(5) . . ?
N11 C58 C57 122.2(7) . . ?
N12 C64 C63 122.9(6) . . ?
C64 C63 C62 119.4(6) . . ?
C61 C62 C63 118.8(6) . . ?
N11 C54 C55 122.3(6) . . ?
N11 C54 C53 116.3(5) . . ?
C55 C54 C53 121.4(6) . . ?
C62 C61 C60 118.8(6) . . ?
N12 C60 C61 122.7(6) . . ?
N12 C60 C59 114.9(5) . . ?
C61 C60 C59 122.2(6) . . ?
N10 C53 C54 109.5(5) . . ?
C55 C56 C57 118.6(7) . . ?
C58 C57 C56 119.7(7) . . ?
N10 C59 C60 111.8(5) . . ?
C56 C55 C54 118.5(7) . . ?

_diffrn_measured_fraction_theta_max 0.914
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.914
_refine_diff_density_max         1.413
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.179
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_R2676P
_database_code_depnum_ccdc_archive 'CCDC 1034091'
_audit_update_record             
;
2014-11-13 deposited with the CCDC.
2014-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Ni2(LClO-bdpa)(CH3OH)2Cl2]PF6'
_chemical_formula_moiety         'C34 H38 Cl3 N6 Ni2 O3, F6 P'
_chemical_formula_sum            'C34 H38 Cl3 F6 N6 Ni2 O3 P'
_chemical_formula_weight         947.40

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_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                   13.4024(5)
_cell_length_b                   18.0346(7)
_cell_length_c                   32.6751(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.282(2)
_cell_angle_gamma                90.00
_cell_volume                     7815.4(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4000
_cell_measurement_theta_min      2.00
_cell_measurement_theta_max      26.00

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3872
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7316
_exptl_absorpt_correction_T_max  0.8310
_exptl_absorpt_process_details   SADABS

_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       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            64869
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         27.00
_reflns_number_total             8523
_reflns_number_gt                6780
_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    ?
_computing_publication_material  ?

_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)+(0.0689P)²+9.4664P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8523
_refine_ls_number_parameters     504
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.1086
_refine_ls_wR_factor_gt          0.0960
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      1.005
_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 0.14717(2) 0.439110(16) 0.104098(9) 0.02228(9) Uani 1 1 d . . .
Ni2 Ni 0.02469(3) 0.246844(16) 0.064991(9) 0.02844(10) Uani 1 1 d . . .
Cl1 Cl 0.19566(5) 0.43756(3) 0.036970(17) 0.02862(15) Uani 1 1 d . . .
Cl2 Cl -0.11951(5) 0.32017(3) 0.04386(2) 0.03642(17) Uani 1 1 d . . .
P1 P 0.75535(6) 0.43981(4) 0.17427(2) 0.03026(16) Uani 1 1 d . . .
F6 F 0.65949(13) 0.44887(9) 0.13954(5) 0.0430(4) Uani 1 1 d . . .
F5 F 0.84990(14) 0.43058(12) 0.20940(5) 0.0595(6) Uani 1 1 d . . .
F4 F 0.81853(15) 0.40295(11) 0.14217(6) 0.0545(5) Uani 1 1 d . . .
F3 F 0.79558(15) 0.51857(10) 0.16252(8) 0.0685(7) Uani 1 1 d . . .
F1 F 0.71525(16) 0.36015(12) 0.18482(8) 0.0751(7) Uani 1 1 d . . .
F2 F 0.69251(16) 0.47676(16) 0.20624(6) 0.0833(8) Uani 1 1 d . . .
O1 O 0.11092(13) 0.32470(9) 0.10548(5) 0.0271(4) Uani 1 1 d . . .
O2 O -0.00530(13) 0.45041(9) 0.08324(5) 0.0267(4) Uani 1 1 d D . .
H92 H -0.035(2) 0.4098(9) 0.0761(9) 0.040 Uiso 1 1 d D . .
O3 O 0.10413(15) 0.28865(10) 0.01919(5) 0.0342(4) Uani 1 1 d D . .
H93 H 0.128(2) 0.3317(8) 0.0249(10) 0.051 Uiso 1 1 d D . .
Cl3 Cl 0.30648(7) 0.19088(4) 0.26070(2) 0.0481(2) Uani 1 1 d . . .
N3 N 0.29142(16) 0.42004(11) 0.13420(6) 0.0257(4) Uani 1 1 d . . .
N6 N -0.02760(17) 0.20285(11) 0.11550(6) 0.0302(5) Uani 1 1 d . . .
N5 N -0.02398(18) 0.16345(11) 0.02132(6) 0.0316(5) Uani 1 1 d . . .
N4 N 0.13698(18) 0.16575(11) 0.07913(6) 0.0300(5) Uani 1 1 d . . .
N2 N 0.15062(15) 0.55472(11) 0.10833(6) 0.0240(4) Uani 1 1 d . . .
N1 N 0.12064(15) 0.45603(11) 0.16542(6) 0.0231(4) Uani 1 1 d . . .
C5 C 0.2633(2) 0.20022(14) 0.17782(8) 0.0349(6) Uani 1 1 d . . .
H5 H 0.3066 0.1586 0.1774 0.042 Uiso 1 1 calc R . .
C1 C 0.1536(2) 0.29357(13) 0.14132(7) 0.0267(5) Uani 1 1 d . . .
C2 C 0.1358(2) 0.32251(13) 0.17951(7) 0.0280(6) Uani 1 1 d . . .
C4 C 0.2457(2) 0.23002(15) 0.21469(8) 0.0363(7) Uani 1 1 d . . .
C10 C 0.08796(19) 0.65639(13) 0.14325(8) 0.0284(6) Uani 1 1 d . . .
H10 H 0.0506 0.6743 0.1638 0.034 Uiso 1 1 calc R . .
C6 C 0.2170(2) 0.23164(14) 0.14071(7) 0.0306(6) Uani 1 1 d . . .
C9 C 0.09943(18) 0.58087(13) 0.13768(7) 0.0242(5) Uani 1 1 d . . .
C7 C 0.0705(2) 0.38976(13) 0.18060(7) 0.0265(5) Uani 1 1 d . . .
H7A H 0.0049 0.3814 0.1630 0.032 Uiso 1 1 calc R . .
H7B H 0.0576 0.3986 0.2093 0.032 Uiso 1 1 calc R . .
C3 C 0.1826(2) 0.29010(14) 0.21627(7) 0.0308(6) Uani 1 1 d . . .
H3 H 0.1710 0.3094 0.2422 0.037 Uiso 1 1 calc R . .
C17 C 0.4677(2) 0.37798(18) 0.18348(9) 0.0428(7) Uani 1 1 d . . .
H17 H 0.5283 0.3634 0.2003 0.051 Uiso 1 1 calc R . .
C16 C 0.3917(2) 0.41069(16) 0.20077(8) 0.0360(6) Uani 1 1 d . . .
H16 H 0.3986 0.4189 0.2298 0.043 Uiso 1 1 calc R . .
C8 C 0.05695(19) 0.52304(13) 0.16390(7) 0.0265(5) Uani 1 1 d . . .
H8A H 0.0562 0.5424 0.1922 0.032 Uiso 1 1 calc R . .
H8B H -0.0131 0.5108 0.1518 0.032 Uiso 1 1 calc R . .
C15 C 0.3038(2) 0.43183(13) 0.17517(8) 0.0274(5) Uani 1 1 d . . .
C19 C 0.3662(2) 0.38749(14) 0.11782(8) 0.0315(6) Uani 1 1 d . . .
H19 H 0.3574 0.3786 0.0889 0.038 Uiso 1 1 calc R . .
C13 C 0.19131(19) 0.60263(13) 0.08413(8) 0.0265(5) Uani 1 1 d . . .
H13 H 0.2267 0.5836 0.0632 0.032 Uiso 1 1 calc R . .
C11 C 0.1318(2) 0.70536(14) 0.11838(9) 0.0320(6) Uani 1 1 d . . .
H11 H 0.1258 0.7573 0.1221 0.038 Uiso 1 1 calc R . .
C14 C 0.21904(19) 0.47040(14) 0.19160(7) 0.0277(6) Uani 1 1 d . . .
H14A H 0.2157 0.4531 0.2201 0.033 Uiso 1 1 calc R . .
H14B H 0.2322 0.5244 0.1927 0.033 Uiso 1 1 calc R . .
C18 C 0.4551(2) 0.36643(17) 0.14119(9) 0.0399(7) Uani 1 1 d . . .
H18 H 0.5073 0.3443 0.1285 0.048 Uiso 1 1 calc R . .
C12 C 0.18386(19) 0.67845(14) 0.08832(8) 0.0308(6) Uani 1 1 d . . .
H12 H 0.2140 0.7112 0.0709 0.037 Uiso 1 1 calc R . .
C20 C 0.2323(2) 0.19834(14) 0.10009(7) 0.0314(6) Uani 1 1 d . . .
H20A H 0.2559 0.2371 0.0823 0.038 Uiso 1 1 calc R . .
H20B H 0.2848 0.1594 0.1047 0.038 Uiso 1 1 calc R . .
C24 C -0.0493(2) 0.07415(13) -0.04802(8) 0.0341(7) Uani 1 1 d . . .
H24 H -0.0571 0.0451 -0.0725 0.041 Uiso 1 1 calc R . .
C26 C -0.1140(2) 0.15853(14) -0.00293(8) 0.0338(6) Uani 1 1 d . . .
H26 H -0.1691 0.1863 0.0043 0.041 Uiso 1 1 calc R . .
C23 C 0.0428(2) 0.07579(13) -0.02238(7) 0.0313(6) Uani 1 1 d . . .
H23 H 0.0975 0.0459 -0.0281 0.038 Uiso 1 1 calc R . .
C29 C 0.0070(2) 0.11271(16) 0.16917(8) 0.0412(7) Uani 1 1 d . . .
H29 H 0.0433 0.0701 0.1800 0.049 Uiso 1 1 calc R . .
C22 C 0.0527(2) 0.12228(13) 0.01185(7) 0.0300(6) Uani 1 1 d . . .
C28 C 0.0234(2) 0.14301(13) 0.13159(8) 0.0325(6) Uani 1 1 d . . .
C21 C 0.1522(2) 0.13158(14) 0.03933(7) 0.0322(6) Uani 1 1 d . . .
H21A H 0.1849 0.0826 0.0445 0.039 Uiso 1 1 calc R . .
H21B H 0.1972 0.1634 0.0253 0.039 Uiso 1 1 calc R . .
C25 C -0.1290(2) 0.11450(14) -0.03793(8) 0.0344(6) Uani 1 1 d . . .
H25 H -0.1931 0.1122 -0.0546 0.041 Uiso 1 1 calc R . .
C27 C 0.0954(2) 0.10995(13) 0.10536(8) 0.0351(7) Uani 1 1 d . . .
H27A H 0.1517 0.0860 0.1236 0.042 Uiso 1 1 calc R . .
H27B H 0.0600 0.0711 0.0874 0.042 Uiso 1 1 calc R . .
C31 C -0.1134(2) 0.20822(17) 0.17432(9) 0.0420(7) Uani 1 1 d . . .
H31 H -0.1609 0.2322 0.1888 0.050 Uiso 1 1 calc R . .
C30 C -0.0627(2) 0.14559(18) 0.19052(9) 0.0447(7) Uani 1 1 d . . .
H30 H -0.0757 0.1255 0.2161 0.054 Uiso 1 1 calc R . .
C32 C -0.0939(2) 0.23505(14) 0.13693(8) 0.0343(6) Uani 1 1 d . . .
H32 H -0.1287 0.2781 0.1258 0.041 Uiso 1 1 calc R . .
C33 C -0.0523(2) 0.50545(14) 0.05542(8) 0.0340(6) Uani 1 1 d . . .
H33A H -0.0792 0.5451 0.0712 0.051 Uiso 1 1 calc R . .
H33B H -0.1074 0.4828 0.0366 0.051 Uiso 1 1 calc R . .
H33C H -0.0025 0.5262 0.0394 0.051 Uiso 1 1 calc R . .
C34 C 0.0599(3) 0.29879(16) -0.02311(8) 0.0446(8) Uani 1 1 d . . .
H34A H 0.0533 0.2506 -0.0371 0.067 Uiso 1 1 calc R . .
H34B H 0.1031 0.3313 -0.0370 0.067 Uiso 1 1 calc R . .
H34C H -0.0069 0.3214 -0.0241 0.067 Uiso 1 1 calc R . .


_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 N3 2.068(2) . ?
Ni1 O2 2.0690(17) . ?
Ni1 N2 2.0896(19) . ?
Ni1 N1 2.107(2) . ?
Ni1 O1 2.1217(16) . ?
Ni1 Cl1 2.3759(7) . ?
Ni2 N6 2.044(2) . ?
Ni2 O3 2.098(2) . ?
Ni2 N4 2.102(2) . ?
Ni2 N5 2.111(2) . ?
Ni2 O1 2.1487(16) . ?
Ni2 Cl2 2.3614(7) . ?
P1 F2 1.581(2) . ?
P1 F3 1.586(2) . ?
P1 F4 1.5857(19) . ?
P1 F1 1.589(2) . ?
P1 F5 1.5913(17) . ?
P1 F6 1.5954(16) . ?
O1 C1 1.349(3) . ?
O2 C33 1.430(3) . ?
O3 C34 1.435(3) . ?
Cl3 C4 1.752(2) . ?
N3 C19 1.338(3) . ?
N3 C15 1.342(3) . ?
N6 C32 1.340(4) . ?
N6 C28 1.343(3) . ?
N5 C22 1.339(4) . ?
N5 C26 1.347(3) . ?
N4 C21 1.479(3) . ?
N4 C27 1.482(4) . ?
N4 C20 1.482(3) . ?
N2 C13 1.339(3) . ?
N2 C9 1.342(3) . ?
N1 C8 1.476(3) . ?
N1 C14 1.488(3) . ?
N1 C7 1.491(3) . ?
C5 C4 1.370(4) . ?
C5 C6 1.400(3) . ?
C5 H5 0.9500 . ?
C1 C2 1.404(3) . ?
C1 C6 1.406(4) . ?
C2 C3 1.401(3) . ?
C2 C7 1.499(3) . ?
C4 C3 1.380(4) . ?
C10 C11 1.387(4) . ?
C10 C9 1.386(3) . ?
C10 H10 0.9500 . ?
C6 C20 1.498(3) . ?
C9 C8 1.512(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C3 H3 0.9500 . ?
C17 C16 1.368(4) . ?
C17 C18 1.384(4) . ?
C17 H17 0.9500 . ?
C16 C15 1.396(3) . ?
C16 H16 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C15 C14 1.496(4) . ?
C19 C18 1.374(4) . ?
C19 H19 0.9500 . ?
C13 C12 1.379(3) . ?
C13 H13 0.9500 . ?
C11 C12 1.373(4) . ?
C11 H11 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C18 H18 0.9500 . ?
C12 H12 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C24 C25 1.372(4) . ?
C24 C23 1.388(4) . ?
C24 H24 0.9500 . ?
C26 C25 1.383(4) . ?
C26 H26 0.9500 . ?
C23 C22 1.389(3) . ?
C23 H23 0.9500 . ?
C29 C30 1.378(4) . ?
C29 C28 1.390(4) . ?
C29 H29 0.9500 . ?
C22 C21 1.506(4) . ?
C28 C27 1.503(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C25 H25 0.9500 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C31 C32 1.374(4) . ?
C31 C30 1.384(4) . ?
C31 H31 0.9500 . ?
C30 H30 0.9500 . ?
C32 H32 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 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
N3 Ni1 O2 169.90(8) . . ?
N3 Ni1 N2 97.14(8) . . ?
O2 Ni1 N2 86.26(7) . . ?
N3 Ni1 N1 81.14(8) . . ?
O2 Ni1 N1 90.28(7) . . ?
N2 Ni1 N1 78.33(8) . . ?
N3 Ni1 O1 91.69(7) . . ?
O2 Ni1 O1 83.37(6) . . ?
N2 Ni1 O1 166.37(8) . . ?
N1 Ni1 O1 92.87(7) . . ?
N3 Ni1 Cl1 94.35(6) . . ?
O2 Ni1 Cl1 94.91(5) . . ?
N2 Ni1 Cl1 93.81(6) . . ?
N1 Ni1 Cl1 170.29(6) . . ?
O1 Ni1 Cl1 95.86(5) . . ?
N6 Ni2 O3 169.69(8) . . ?
N6 Ni2 N4 82.55(9) . . ?
O3 Ni2 N4 89.19(8) . . ?
N6 Ni2 N5 99.25(8) . . ?
O3 Ni2 N5 85.00(8) . . ?
N4 Ni2 N5 78.14(8) . . ?
N6 Ni2 O1 88.46(7) . . ?
O3 Ni2 O1 85.48(7) . . ?
N4 Ni2 O1 90.85(7) . . ?
N5 Ni2 O1 165.53(9) . . ?
N6 Ni2 Cl2 95.28(6) . . ?
O3 Ni2 Cl2 93.91(5) . . ?
N4 Ni2 Cl2 169.72(6) . . ?
N5 Ni2 Cl2 92.35(6) . . ?
O1 Ni2 Cl2 99.15(5) . . ?
F2 P1 F3 90.83(15) . . ?
F2 P1 F4 179.85(14) . . ?
F3 P1 F4 89.01(12) . . ?
F2 P1 F1 90.50(15) . . ?
F3 P1 F1 178.46(14) . . ?
F4 P1 F1 89.65(12) . . ?
F2 P1 F5 90.69(10) . . ?
F3 P1 F5 90.30(11) . . ?
F4 P1 F5 89.30(10) . . ?
F1 P1 F5 90.46(12) . . ?
F2 P1 F6 88.61(10) . . ?
F3 P1 F6 90.17(9) . . ?
F4 P1 F6 91.40(10) . . ?
F1 P1 F6 89.08(11) . . ?
F5 P1 F6 179.16(11) . . ?
C1 O1 Ni1 110.70(13) . . ?
C1 O1 Ni2 112.68(14) . . ?
Ni1 O1 Ni2 136.63(7) . . ?
C33 O2 Ni1 127.00(16) . . ?
C34 O3 Ni2 123.45(19) . . ?
C19 N3 C15 118.5(2) . . ?
C19 N3 Ni1 125.84(16) . . ?
C15 N3 Ni1 114.89(17) . . ?
C32 N6 C28 118.8(2) . . ?
C32 N6 Ni2 125.73(17) . . ?
C28 N6 Ni2 114.44(19) . . ?
C22 N5 C26 118.6(2) . . ?
C22 N5 Ni2 112.25(16) . . ?
C26 N5 Ni2 127.43(18) . . ?
C21 N4 C27 109.68(19) . . ?
C21 N4 C20 110.7(2) . . ?
C27 N4 C20 111.92(19) . . ?
C21 N4 Ni2 106.35(14) . . ?
C27 N4 Ni2 106.41(17) . . ?
C20 N4 Ni2 111.60(14) . . ?
C13 N2 C9 119.2(2) . . ?
C13 N2 Ni1 127.71(17) . . ?
C9 N2 Ni1 112.90(16) . . ?
C8 N1 C14 109.71(18) . . ?
C8 N1 C7 112.4(2) . . ?
C14 N1 C7 110.67(18) . . ?
C8 N1 Ni1 105.22(14) . . ?
C14 N1 Ni1 108.36(15) . . ?
C7 N1 Ni1 110.25(14) . . ?
C4 C5 C6 119.5(2) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
O1 C1 C2 120.8(2) . . ?
O1 C1 C6 120.0(2) . . ?
C2 C1 C6 119.2(2) . . ?
C3 C2 C1 119.7(2) . . ?
C3 C2 C7 120.5(2) . . ?
C1 C2 C7 119.8(2) . . ?
C5 C4 C3 121.7(2) . . ?
C5 C4 Cl3 118.6(2) . . ?
C3 C4 Cl3 119.7(2) . . ?
C11 C10 C9 119.0(2) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C5 C6 C1 120.2(2) . . ?
C5 C6 C20 120.3(2) . . ?
C1 C6 C20 119.4(2) . . ?
N2 C9 C10 121.1(2) . . ?
N2 C9 C8 115.8(2) . . ?
C10 C9 C8 123.1(2) . . ?
N1 C7 C2 110.4(2) . . ?
N1 C7 H7A 109.6 . . ?
C2 C7 H7A 109.6 . . ?
N1 C7 H7B 109.6 . . ?
C2 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C4 C3 C2 119.8(2) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C16 C17 C18 119.1(2) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C17 C16 C15 119.0(2) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
N1 C8 C9 108.7(2) . . ?
N1 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
N1 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.3 . . ?
N3 C15 C16 121.8(2) . . ?
N3 C15 C14 116.1(2) . . ?
C16 C15 C14 122.1(2) . . ?
N3 C19 C18 122.6(2) . . ?
N3 C19 H19 118.7 . . ?
C18 C19 H19 118.7 . . ?
N2 C13 C12 122.7(3) . . ?
N2 C13 H13 118.7 . . ?
C12 C13 H13 118.7 . . ?
C12 C11 C10 119.7(2) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
N1 C14 C15 111.64(19) . . ?
N1 C14 H14A 109.3 . . ?
C15 C14 H14A 109.3 . . ?
N1 C14 H14B 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C19 C18 C17 119.0(3) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C11 C12 C13 118.2(3) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 H12 120.9 . . ?
N4 C20 C6 110.5(2) . . ?
N4 C20 H20A 109.6 . . ?
C6 C20 H20A 109.6 . . ?
N4 C20 H20B 109.6 . . ?
C6 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C25 C24 C23 119.9(2) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
N5 C26 C25 122.4(3) . . ?
N5 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
C22 C23 C24 118.2(3) . . ?
C22 C23 H23 120.9 . . ?
C24 C23 H23 120.9 . . ?
C30 C29 C28 118.9(3) . . ?
C30 C29 H29 120.6 . . ?
C28 C29 H29 120.6 . . ?
N5 C22 C23 122.2(2) . . ?
N5 C22 C21 116.3(2) . . ?
C23 C22 C21 121.4(3) . . ?
N6 C28 C29 121.7(3) . . ?
N6 C28 C27 115.3(2) . . ?
C29 C28 C27 122.9(2) . . ?
N4 C21 C22 110.4(2) . . ?
N4 C21 H21A 109.6 . . ?
C22 C21 H21A 109.6 . . ?
N4 C21 H21B 109.6 . . ?
C22 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C24 C25 C26 118.5(3) . . ?
C24 C25 H25 120.7 . . ?
C26 C25 H25 120.7 . . ?
N4 C27 C28 112.7(2) . . ?
N4 C27 H27A 109.0 . . ?
C28 C27 H27A 109.0 . . ?
N4 C27 H27B 109.0 . . ?
C28 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?
C32 C31 C30 118.8(3) . . ?
C32 C31 H31 120.6 . . ?
C30 C31 H31 120.6 . . ?
C29 C30 C31 119.3(3) . . ?
C29 C30 H30 120.4 . . ?
C31 C30 H30 120.4 . . ?
N6 C32 C31 122.5(3) . . ?
N6 C32 H32 118.7 . . ?
C31 C32 H32 118.7 . . ?
O2 C33 H33A 109.5 . . ?
O2 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O2 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O3 C34 H34A 109.5 . . ?
O3 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O3 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 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
O1 C1 C2 C3 -178.7(2) . . . . ?
C6 C1 C2 C3 1.0(4) . . . . ?
O1 C1 C2 C7 -1.3(4) . . . . ?
C6 C1 C2 C7 178.4(2) . . . . ?
C6 C5 C4 C3 0.6(5) . . . . ?
C6 C5 C4 Cl3 -178.7(2) . . . . ?
C4 C5 C6 C1 0.4(4) . . . . ?
C4 C5 C6 C20 -177.9(3) . . . . ?
O1 C1 C6 C5 178.5(2) . . . . ?
C2 C1 C6 C5 -1.2(4) . . . . ?
O1 C1 C6 C20 -3.2(4) . . . . ?
C2 C1 C6 C20 177.1(2) . . . . ?
C13 N2 C9 C10 0.1(3) . . . . ?
C13 N2 C9 C8 -179.4(2) . . . . ?
C11 C10 C9 N2 -1.1(3) . . . . ?
C11 C10 C9 C8 178.4(2) . . . . ?
C8 N1 C7 C2 177.08(18) . . . . ?
C14 N1 C7 C2 -59.9(2) . . . . ?
C3 C2 C7 N1 109.9(3) . . . . ?
C1 C2 C7 N1 -67.4(3) . . . . ?
C5 C4 C3 C2 -0.8(5) . . . . ?
Cl3 C4 C3 C2 178.5(2) . . . . ?
C1 C2 C3 C4 0.0(4) . . . . ?
C7 C2 C3 C4 -177.4(3) . . . . ?
C18 C17 C16 C15 -0.3(5) . . . . ?
C14 N1 C8 C9 71.9(2) . . . . ?
C7 N1 C8 C9 -164.52(18) . . . . ?
N2 C9 C8 N1 27.6(3) . . . . ?
C10 C9 C8 N1 -151.8(2) . . . . ?
C19 N3 C15 C16 -0.4(4) . . . . ?
C19 N3 C15 C14 178.3(2) . . . . ?
C17 C16 C15 N3 0.9(4) . . . . ?
C17 C16 C15 C14 -177.7(3) . . . . ?
C15 N3 C19 C18 -0.7(4) . . . . ?
C9 N2 C13 C12 0.7(3) . . . . ?
C9 C10 C11 C12 1.2(4) . . . . ?
C8 N1 C14 C15 -144.2(2) . . . . ?
C7 N1 C14 C15 91.2(2) . . . . ?
N3 C15 C14 N1 28.2(3) . . . . ?
C16 C15 C14 N1 -153.2(2) . . . . ?
N3 C19 C18 C17 1.2(5) . . . . ?
C16 C17 C18 C19 -0.7(5) . . . . ?
C10 C11 C12 C13 -0.4(4) . . . . ?
N2 C13 C12 C11 -0.6(4) . . . . ?
C21 N4 C20 C6 -178.98(19) . . . . ?
C27 N4 C20 C6 -56.3(3) . . . . ?
C5 C6 C20 N4 112.4(3) . . . . ?
C1 C6 C20 N4 -65.9(3) . . . . ?
C22 N5 C26 C25 -2.2(4) . . . . ?
C25 C24 C23 C22 -3.7(4) . . . . ?
C26 N5 C22 C23 1.0(4) . . . . ?
C26 N5 C22 C21 178.4(2) . . . . ?
C24 C23 C22 N5 1.9(4) . . . . ?
C24 C23 C22 C21 -175.3(2) . . . . ?
C32 N6 C28 C29 1.8(4) . . . . ?
C32 N6 C28 C27 179.4(2) . . . . ?
C30 C29 C28 N6 -0.6(4) . . . . ?
C30 C29 C28 C27 -178.1(3) . . . . ?
C27 N4 C21 C22 75.4(3) . . . . ?
C20 N4 C21 C22 -160.7(2) . . . . ?
N5 C22 C21 N4 18.8(3) . . . . ?
C23 C22 C21 N4 -163.9(2) . . . . ?
C23 C24 C25 C26 2.6(4) . . . . ?
N5 C26 C25 C24 0.4(4) . . . . ?
C21 N4 C27 C28 -145.7(2) . . . . ?
C20 N4 C27 C28 91.1(3) . . . . ?
N6 C28 C27 N4 29.6(3) . . . . ?
C29 C28 C27 N4 -152.7(3) . . . . ?
C28 C29 C30 C31 -0.8(4) . . . . ?
C32 C31 C30 C29 1.1(4) . . . . ?
C28 N6 C32 C31 -1.5(4) . . . . ?
C30 C31 C32 N6 0.0(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.086
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_r2676c
_database_code_depnum_ccdc_archive 'CCDC 1034092'
_audit_update_record             
;
2014-11-13 deposited with the CCDC.
2014-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Ni2(LClO-tmpa)Cl2(H2O)(MeOH)]ClO4.xH2O'
_chemical_formula_moiety         '4(C33 H36 Cl3 N6 Ni2 O3), 4(Cl O4), 5(O)'
_chemical_formula_sum            'C132 H144 Cl16 N24 Ni8 O33'
_chemical_formula_weight         3631.43

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   10.3560(5)
_cell_length_b                   19.7894(9)
_cell_length_c                   19.0876(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.752(2)
_cell_angle_gamma                90.00
_cell_volume                     3884.7(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4000
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      28.00

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1864
_exptl_absorpt_coefficient_mu    1.301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6733
_exptl_absorpt_correction_T_max  0.7628
_exptl_absorpt_process_details   SADABS

_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       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            50341
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.58
_diffrn_reflns_theta_max         29.04
_reflns_number_total             10297
_reflns_number_gt                7385
_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 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0614P)²+6.4066P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10297
_refine_ls_number_parameters     515
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1381
_refine_ls_wR_factor_gt          0.1203
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.047
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.71016(4) 0.194577(19) 0.92236(2) 0.02527(10) Uani 1 d . . .
Ni2 Ni 1.06436(4) 0.27094(2) 0.97014(2) 0.02657(11) Uani 1 d . . .
Cl3 Cl 1.09688(9) 0.15641(5) 1.00339(5) 0.0402(2) Uani 1 d . . .
Cl2 Cl 0.72849(9) 0.19732(4) 1.04793(4) 0.03467(19) Uani 1 d . . .
Cl1 Cl 0.79773(14) 0.43238(6) 0.65723(6) 0.0623(3) Uani 1 d . . .
O1 O 0.8757(2) 0.25786(10) 0.90855(12) 0.0250(4) Uani 1 d . . .
N2 N 0.5553(3) 0.12472(13) 0.91659(15) 0.0310(6) Uani 1 d . . .
N3 N 0.5999(2) 0.28072(13) 0.90513(14) 0.0257(5) Uani 1 d . . .
N1 N 0.6638(3) 0.18361(12) 0.81263(15) 0.0261(5) Uani 1 d . . .
N6 N 1.1437(2) 0.26300(14) 0.87747(15) 0.0278(6) Uani 1 d . . .
N4 N 1.0642(2) 0.37435(13) 0.94712(14) 0.0263(5) Uani 1 d . . .
N5 N 1.2363(3) 0.30403(15) 1.03092(15) 0.0313(6) Uani 1 d . . .
C2 C 0.8151(3) 0.27101(15) 0.78395(17) 0.0261(6) Uani 1 d . . .
C6 C 0.8785(3) 0.36813(15) 0.85614(17) 0.0258(6) Uani 1 d . . .
C5 C 0.8600(3) 0.40895(16) 0.79689(18) 0.0311(7) Uani 1 d . . .
H5 H 0.8749 0.4562 0.8011 0.037 Uiso 1 calc R . .
C7 C 0.7805(3) 0.19754(15) 0.77635(18) 0.0281(7) Uani 1 d . . .
H7A H 0.7623 0.1858 0.7257 0.034 Uiso 1 calc R . .
H7B H 0.8543 0.1695 0.7974 0.034 Uiso 1 calc R . .
C3 C 0.7969(3) 0.31231(17) 0.72531(18) 0.0313(7) Uani 1 d . . .
H3 H 0.7685 0.2935 0.6803 0.038 Uiso 1 calc R . .
C8 C 0.6214(3) 0.11224(15) 0.80060(19) 0.0310(7) Uani 1 d . . .
H8A H 0.6980 0.0819 0.8062 0.037 Uiso 1 calc R . .
H8B H 0.5770 0.1069 0.7521 0.037 Uiso 1 calc R . .
C4 C 0.8199(4) 0.38091(17) 0.73182(19) 0.0341(7) Uani 1 d . . .
C1 C 0.8572(3) 0.29751(14) 0.85142(17) 0.0232(6) Uani 1 d . . .
C13 C 0.4788(4) 0.11053(17) 0.9663(2) 0.0373(8) Uani 1 d . . .
H13 H 0.4961 0.1318 1.0111 0.045 Uiso 1 calc R . .
C10 C 0.4297(4) 0.04858(17) 0.8388(2) 0.0378(8) Uani 1 d . . .
H10 H 0.4147 0.0273 0.7940 0.045 Uiso 1 calc R . .
C9 C 0.5303(3) 0.09395(15) 0.85317(19) 0.0297(7) Uani 1 d . . .
C12 C 0.3749(4) 0.06593(19) 0.9551(2) 0.0422(9) Uani 1 d . . .
H12 H 0.3214 0.0574 0.9914 0.051 Uiso 1 calc R . .
C19 C 0.5964(3) 0.33205(16) 0.95095(18) 0.0280(6) Uani 1 d . . .
H19 H 0.6302 0.3252 0.9989 0.034 Uiso 1 calc R . .
C17 C 0.4984(3) 0.40520(17) 0.8611(2) 0.0346(8) Uani 1 d . . .
H17 H 0.4628 0.4477 0.8460 0.042 Uiso 1 calc R . .
C14 C 0.5541(3) 0.23002(16) 0.78981(18) 0.0291(7) Uani 1 d . . .
H14A H 0.4710 0.2053 0.7899 0.035 Uiso 1 calc R . .
H14B H 0.5607 0.2452 0.7409 0.035 Uiso 1 calc R . .
C16 C 0.5038(3) 0.35241(17) 0.81299(19) 0.0305(7) Uani 1 d . . .
H16 H 0.4738 0.3587 0.7645 0.037 Uiso 1 calc R . .
C15 C 0.5535(3) 0.29090(15) 0.83722(18) 0.0265(6) Uani 1 d . . .
C18 C 0.5450(3) 0.39483(16) 0.93045(19) 0.0318(7) Uani 1 d . . .
H18 H 0.5422 0.4301 0.9641 0.038 Uiso 1 calc R . .
C22 C 1.2361(3) 0.37058(18) 1.04526(17) 0.0319(7) Uani 1 d . . .
C20 C 0.9295(3) 0.39873(15) 0.92541(17) 0.0265(6) Uani 1 d . . .
H20A H 0.9294 0.4486 0.9213 0.032 Uiso 1 calc R . .
H20B H 0.8728 0.3860 0.9616 0.032 Uiso 1 calc R . .
C26 C 1.3390(3) 0.2670(2) 1.05756(19) 0.0374(8) Uani 1 d . . .
H26 H 1.3405 0.2202 1.0468 0.045 Uiso 1 calc R . .
C21 C 1.1199(3) 0.40871(17) 1.01282(18) 0.0323(7) Uani 1 d . . .
H21A H 1.0540 0.4110 1.0464 0.039 Uiso 1 calc R . .
H21B H 1.1453 0.4554 1.0020 0.039 Uiso 1 calc R . .
C23 C 1.3371(4) 0.4015(2) 1.0883(2) 0.0419(9) Uani 1 d . . .
H23 H 1.3343 0.4485 1.0981 0.050 Uiso 1 calc R . .
C24 C 1.4415(4) 0.3626(3) 1.1164(2) 0.0491(11) Uani 1 d . . .
H24 H 1.5109 0.3825 1.1465 0.059 Uiso 1 calc R . .
C25 C 1.4435(4) 0.2949(3) 1.1003(2) 0.0477(11) Uani 1 d . . .
H25 H 1.5153 0.2675 1.1182 0.057 Uiso 1 calc R . .
C28 C 1.1578(3) 0.32258(17) 0.84520(18) 0.0287(7) Uani 1 d . . .
C27 C 1.1506(3) 0.38437(17) 0.89084(18) 0.0300(7) Uani 1 d . . .
H27A H 1.2392 0.3958 0.9130 0.036 Uiso 1 calc R . .
H27B H 1.1180 0.4229 0.8608 0.036 Uiso 1 calc R . .
C30 C 1.2015(3) 0.2665(2) 0.73986(19) 0.0372(8) Uani 1 d . . .
H30 H 1.2217 0.2677 0.6926 0.045 Uiso 1 calc R . .
C29 C 1.1848(3) 0.32627(19) 0.77619(19) 0.0341(7) Uani 1 d . . .
H29 H 1.1920 0.3688 0.7539 0.041 Uiso 1 calc R . .
C32 C 1.1582(3) 0.20552(18) 0.84100(19) 0.0316(7) Uani 1 d . . .
H32 H 1.1471 0.1634 0.8634 0.038 Uiso 1 calc R . .
C31 C 1.1883(3) 0.20570(19) 0.7730(2) 0.0354(8) Uani 1 d . . .
H31 H 1.1999 0.1644 0.7491 0.042 Uiso 1 calc R . .
C11 C 0.3506(4) 0.03438(19) 0.8911(2) 0.0445(9) Uani 1 d . . .
H11 H 0.2807 0.0032 0.8825 0.053 Uiso 1 calc R . .
Cl4 Cl 0.28623(8) 0.06595(4) 0.62832(4) 0.02829(17) Uani 1 d . . .
O4 O 0.4230(3) 0.05014(14) 0.63971(15) 0.0448(6) Uani 1 d . . .
O5 O 0.2678(3) 0.13799(13) 0.62378(17) 0.0516(7) Uani 1 d . . .
O6 O 0.2285(3) 0.03538(15) 0.56378(14) 0.0529(8) Uani 1 d . . .
O7 O 0.2240(3) 0.04040(14) 0.68544(13) 0.0422(6) Uani 1 d . . .
O2 O 0.8420(2) 0.11442(11) 0.92275(13) 0.0341(5) Uani 1 d D . .
H90 H 0.9118(9) 0.1345(7) 0.9385(4) 0.051 Uiso 1 d D . .
C39 C 0.8264(5) 0.0523(2) 0.9622(3) 0.0613(13) Uani 1 d . . .
H39A H 0.8266 0.0630 1.0123 0.092 Uiso 1 calc R . .
H39B H 0.8984 0.0215 0.9562 0.092 Uiso 1 calc R . .
H39C H 0.7439 0.0307 0.9444 0.092 Uiso 1 calc R . .
O3 O 0.9711(3) 0.28570(14) 1.06093(17) 0.0487(7) Uani 1 d D . .
H91 H 0.9148(9) 0.2549(7) 1.0528(4) 0.073 Uiso 1 d D . .
H92 H 0.9285(9) 0.3152(7) 1.0806(4) 0.073 Uiso 1 d D . .
O10 O 0.4439(8) 0.4060(5) 0.6369(4) 0.070(2) Uani 0.50 d PU A 1
O11 O 0.4780(14) 0.3484(8) 0.6390(7) 0.067(4) Uani 0.25 d PU B 2
O12 O 0.3791(18) 0.4045(8) 0.6557(8) 0.067(4) Uani 0.25 d PU C 3
O13 O 0.4899(17) 0.5296(8) 0.7094(9) 0.081(4) Uani 0.25 d PU D 4


_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 N3 2.057(3) . ?
Ni1 O2 2.092(2) . ?
Ni1 N1 2.104(3) . ?
Ni1 N2 2.110(3) . ?
Ni1 O1 2.164(2) . ?
Ni1 Cl2 2.3826(9) . ?
Ni2 N6 2.042(3) . ?
Ni2 N4 2.093(3) . ?
Ni2 O3 2.101(3) . ?
Ni2 N5 2.111(3) . ?
Ni2 O1 2.174(2) . ?
Ni2 Cl3 2.3670(10) . ?
Cl1 C4 1.744(4) . ?
O1 C1 1.339(4) . ?
N2 C13 1.336(4) . ?
N2 C9 1.353(4) . ?
N3 C15 1.343(4) . ?
N3 C19 1.344(4) . ?
N1 C14 1.486(4) . ?
N1 C7 1.488(4) . ?
N1 C8 1.489(4) . ?
N6 C28 1.346(4) . ?
N6 C32 1.351(4) . ?
N4 C21 1.483(4) . ?
N4 C20 1.488(4) . ?
N4 C27 1.490(4) . ?
N5 C26 1.342(4) . ?
N5 C22 1.345(5) . ?
C2 C3 1.381(5) . ?
C2 C1 1.411(4) . ?
C2 C7 1.501(4) . ?
C6 C5 1.385(5) . ?
C6 C1 1.416(4) . ?
C6 C20 1.493(4) . ?
C5 C4 1.379(5) . ?
C5 H5 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C3 C4 1.381(5) . ?
C3 H3 0.9500 . ?
C8 C9 1.500(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C13 C12 1.389(5) . ?
C13 H13 0.9500 . ?
C10 C9 1.378(5) . ?
C10 C11 1.393(6) . ?
C10 H10 0.9500 . ?
C12 C11 1.369(6) . ?
C12 H12 0.9500 . ?
C19 C18 1.390(5) . ?
C19 H19 0.9500 . ?
C17 C18 1.370(5) . ?
C17 C16 1.397(5) . ?
C17 H17 0.9500 . ?
C14 C15 1.507(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C16 C15 1.380(5) . ?
C16 H16 0.9500 . ?
C18 H18 0.9500 . ?
C22 C23 1.393(5) . ?
C22 C21 1.492(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C26 C25 1.391(6) . ?
C26 H26 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C23 C24 1.383(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.376(7) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C28 C29 1.380(5) . ?
C28 C27 1.508(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C30 C31 1.373(5) . ?
C30 C29 1.392(5) . ?
C30 H30 0.9500 . ?
C29 H29 0.9500 . ?
C32 C31 1.371(5) . ?
C32 H32 0.9500 . ?
C31 H31 0.9500 . ?
C11 H11 0.9500 . ?
Cl4 O7 1.423(3) . ?
Cl4 O6 1.438(3) . ?
Cl4 O5 1.440(3) . ?
Cl4 O4 1.442(3) . ?
O2 C39 1.460(5) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 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
N3 Ni1 O2 168.17(10) . . ?
N3 Ni1 N1 82.47(10) . . ?
O2 Ni1 N1 89.88(10) . . ?
N3 Ni1 N2 97.51(11) . . ?
O2 Ni1 N2 89.71(10) . . ?
N1 Ni1 N2 78.31(11) . . ?
N3 Ni1 O1 86.19(9) . . ?
O2 Ni1 O1 85.03(9) . . ?
N1 Ni1 O1 91.71(9) . . ?
N2 Ni1 O1 168.75(10) . . ?
N3 Ni1 Cl2 96.83(8) . . ?
O2 Ni1 Cl2 92.23(7) . . ?
N1 Ni1 Cl2 170.22(7) . . ?
N2 Ni1 Cl2 92.15(8) . . ?
O1 Ni1 Cl2 97.98(6) . . ?
N6 Ni2 N4 83.33(11) . . ?
N6 Ni2 O3 174.77(12) . . ?
N4 Ni2 O3 92.75(11) . . ?
N6 Ni2 N5 95.79(10) . . ?
N4 Ni2 N5 78.00(11) . . ?
O3 Ni2 N5 86.75(11) . . ?
N6 Ni2 O1 87.12(9) . . ?
N4 Ni2 O1 91.39(9) . . ?
O3 Ni2 O1 89.52(10) . . ?
N5 Ni2 O1 168.55(10) . . ?
N6 Ni2 Cl3 95.71(8) . . ?
N4 Ni2 Cl3 171.53(8) . . ?
O3 Ni2 Cl3 88.67(9) . . ?
N5 Ni2 Cl3 93.75(9) . . ?
O1 Ni2 Cl3 96.98(6) . . ?
C1 O1 Ni1 113.53(18) . . ?
C1 O1 Ni2 113.81(17) . . ?
Ni1 O1 Ni2 132.64(11) . . ?
C13 N2 C9 118.3(3) . . ?
C13 N2 Ni1 127.7(2) . . ?
C9 N2 Ni1 114.0(2) . . ?
C15 N3 C19 118.7(3) . . ?
C15 N3 Ni1 114.0(2) . . ?
C19 N3 Ni1 125.4(2) . . ?
C14 N1 C7 112.6(3) . . ?
C14 N1 C8 109.9(3) . . ?
C7 N1 C8 110.2(2) . . ?
C14 N1 Ni1 107.77(19) . . ?
C7 N1 Ni1 110.0(2) . . ?
C8 N1 Ni1 106.3(2) . . ?
C28 N6 C32 118.5(3) . . ?
C28 N6 Ni2 113.9(2) . . ?
C32 N6 Ni2 126.3(2) . . ?
C21 N4 C20 110.2(2) . . ?
C21 N4 C27 110.0(2) . . ?
C20 N4 C27 112.3(3) . . ?
C21 N4 Ni2 106.3(2) . . ?
C20 N4 Ni2 110.68(18) . . ?
C27 N4 Ni2 107.19(19) . . ?
C26 N5 C22 118.5(3) . . ?
C26 N5 Ni2 128.3(3) . . ?
C22 N5 Ni2 113.2(2) . . ?
C3 C2 C1 121.2(3) . . ?
C3 C2 C7 119.1(3) . . ?
C1 C2 C7 119.5(3) . . ?
C5 C6 C1 121.2(3) . . ?
C5 C6 C20 119.2(3) . . ?
C1 C6 C20 119.5(3) . . ?
C4 C5 C6 119.9(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
N1 C7 C2 109.4(2) . . ?
N1 C7 H7A 109.8 . . ?
C2 C7 H7A 109.8 . . ?
N1 C7 H7B 109.8 . . ?
C2 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
C2 C3 C4 120.2(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
N1 C8 C9 108.8(3) . . ?
N1 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
N1 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
C5 C4 C3 120.5(3) . . ?
C5 C4 Cl1 119.8(3) . . ?
C3 C4 Cl1 119.7(3) . . ?
O1 C1 C2 121.7(3) . . ?
O1 C1 C6 121.4(3) . . ?
C2 C1 C6 117.0(3) . . ?
N2 C13 C12 122.6(4) . . ?
N2 C13 H13 118.7 . . ?
C12 C13 H13 118.7 . . ?
C9 C10 C11 118.9(4) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
N2 C9 C10 122.2(3) . . ?
N2 C9 C8 114.9(3) . . ?
C10 C9 C8 123.0(3) . . ?
C11 C12 C13 119.0(4) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
N3 C19 C18 122.1(3) . . ?
N3 C19 H19 119.0 . . ?
C18 C19 H19 119.0 . . ?
C18 C17 C16 119.1(3) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
N1 C14 C15 112.0(3) . . ?
N1 C14 H14A 109.2 . . ?
C15 C14 H14A 109.2 . . ?
N1 C14 H14B 109.2 . . ?
C15 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C15 C16 C17 118.8(3) . . ?
C15 C16 H16 120.6 . . ?
C17 C16 H16 120.6 . . ?
N3 C15 C16 122.2(3) . . ?
N3 C15 C14 115.7(3) . . ?
C16 C15 C14 122.1(3) . . ?
C17 C18 C19 119.1(3) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
N5 C22 C23 122.1(3) . . ?
N5 C22 C21 115.5(3) . . ?
C23 C22 C21 122.4(3) . . ?
N4 C20 C6 109.7(2) . . ?
N4 C20 H20A 109.7 . . ?
C6 C20 H20A 109.7 . . ?
N4 C20 H20B 109.7 . . ?
C6 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
N5 C26 C25 122.3(4) . . ?
N5 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
N4 C21 C22 109.5(3) . . ?
N4 C21 H21A 109.8 . . ?
C22 C21 H21A 109.8 . . ?
N4 C21 H21B 109.8 . . ?
C22 C21 H21B 109.8 . . ?
H21A C21 H21B 108.2 . . ?
C24 C23 C22 118.9(4) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
C25 C24 C23 119.1(4) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C24 C25 C26 119.1(4) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
N6 C28 C29 121.9(3) . . ?
N6 C28 C27 115.5(3) . . ?
C29 C28 C27 122.5(3) . . ?
N4 C27 C28 112.5(3) . . ?
N4 C27 H27A 109.1 . . ?
C28 C27 H27A 109.1 . . ?
N4 C27 H27B 109.1 . . ?
C28 C27 H27B 109.1 . . ?
H27A C27 H27B 107.8 . . ?
C31 C30 C29 119.4(3) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C28 C29 C30 118.8(3) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 H29 120.6 . . ?
N6 C32 C31 122.5(3) . . ?
N6 C32 H32 118.7 . . ?
C31 C32 H32 118.7 . . ?
C32 C31 C30 119.0(3) . . ?
C32 C31 H31 120.5 . . ?
C30 C31 H31 120.5 . . ?
C12 C11 C10 119.1(3) . . ?
C12 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
O7 Cl4 O6 109.08(19) . . ?
O7 Cl4 O5 109.20(18) . . ?
O6 Cl4 O5 109.04(18) . . ?
O7 Cl4 O4 109.44(17) . . ?
O6 Cl4 O4 109.87(18) . . ?
O5 Cl4 O4 110.19(18) . . ?
C39 O2 Ni1 121.9(3) . . ?
O2 C39 H39A 109.5 . . ?
O2 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O2 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 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
C1 C6 C5 C4 0.1(5) . . . . ?
C20 C6 C5 C4 176.4(3) . . . . ?
C14 N1 C7 C2 52.3(3) . . . . ?
C8 N1 C7 C2 175.3(3) . . . . ?
C3 C2 C7 N1 -110.2(3) . . . . ?
C1 C2 C7 N1 65.6(4) . . . . ?
C1 C2 C3 C4 0.0(5) . . . . ?
C7 C2 C3 C4 175.7(3) . . . . ?
C14 N1 C8 C9 -71.4(3) . . . . ?
C7 N1 C8 C9 164.0(3) . . . . ?
C6 C5 C4 C3 0.6(5) . . . . ?
C6 C5 C4 Cl1 -179.6(3) . . . . ?
C2 C3 C4 C5 -0.6(5) . . . . ?
C2 C3 C4 Cl1 179.5(3) . . . . ?
C3 C2 C1 O1 -179.7(3) . . . . ?
C7 C2 C1 O1 4.6(4) . . . . ?
C3 C2 C1 C6 0.6(4) . . . . ?
C7 C2 C1 C6 -175.1(3) . . . . ?
C5 C6 C1 O1 179.7(3) . . . . ?
C20 C6 C1 O1 3.4(4) . . . . ?
C5 C6 C1 C2 -0.7(4) . . . . ?
C20 C6 C1 C2 -176.9(3) . . . . ?
C9 N2 C13 C12 -0.3(5) . . . . ?
C13 N2 C9 C10 -0.4(5) . . . . ?
C13 N2 C9 C8 -179.5(3) . . . . ?
C11 C10 C9 N2 0.6(5) . . . . ?
C11 C10 C9 C8 179.6(3) . . . . ?
N1 C8 C9 N2 -32.7(4) . . . . ?
N1 C8 C9 C10 148.3(3) . . . . ?
N2 C13 C12 C11 1.0(6) . . . . ?
C15 N3 C19 C18 0.8(4) . . . . ?
C7 N1 C14 C15 -93.2(3) . . . . ?
C8 N1 C14 C15 143.6(3) . . . . ?
C18 C17 C16 C15 1.4(5) . . . . ?
C19 N3 C15 C16 0.7(4) . . . . ?
C19 N3 C15 C14 -176.8(3) . . . . ?
C17 C16 C15 N3 -1.8(5) . . . . ?
C17 C16 C15 C14 175.6(3) . . . . ?
N1 C14 C15 N3 -31.5(4) . . . . ?
N1 C14 C15 C16 151.0(3) . . . . ?
C16 C17 C18 C19 0.0(5) . . . . ?
N3 C19 C18 C17 -1.2(5) . . . . ?
C26 N5 C22 C23 -1.9(5) . . . . ?
C26 N5 C22 C21 178.9(3) . . . . ?
C21 N4 C20 C6 175.3(3) . . . . ?
C27 N4 C20 C6 52.3(3) . . . . ?
C5 C6 C20 N4 -110.5(3) . . . . ?
C1 C6 C20 N4 65.9(4) . . . . ?
C22 N5 C26 C25 1.2(5) . . . . ?
C20 N4 C21 C22 163.5(3) . . . . ?
C27 N4 C21 C22 -72.2(3) . . . . ?
N5 C22 C21 N4 -27.4(4) . . . . ?
C23 C22 C21 N4 153.4(3) . . . . ?
N5 C22 C23 C24 0.8(5) . . . . ?
C21 C22 C23 C24 179.9(3) . . . . ?
C22 C23 C24 C25 1.0(5) . . . . ?
C23 C24 C25 C26 -1.6(5) . . . . ?
N5 C26 C25 C24 0.5(5) . . . . ?
C32 N6 C28 C29 0.8(5) . . . . ?
C32 N6 C28 C27 -175.4(3) . . . . ?
C21 N4 C27 C28 142.5(3) . . . . ?
C20 N4 C27 C28 -94.3(3) . . . . ?
N6 C28 C27 N4 -30.6(4) . . . . ?
C29 C28 C27 N4 153.2(3) . . . . ?
N6 C28 C29 C30 -1.8(5) . . . . ?
C27 C28 C29 C30 174.1(3) . . . . ?
C31 C30 C29 C28 1.2(5) . . . . ?
C28 N6 C32 C31 0.9(5) . . . . ?
N6 C32 C31 C30 -1.5(5) . . . . ?
C29 C30 C31 C32 0.4(5) . . . . ?
C13 C12 C11 C10 -0.8(6) . . . . ?
C9 C10 C11 C12 0.1(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        29.04
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.623
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.095
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_r2620
_database_code_depnum_ccdc_archive 'CCDC 1034093'
_audit_update_record             
;
2014-11-13 deposited with the CCDC.
2014-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Cu2(LClO-tmpa)Cl2]Pf6.1/2MeOH'
_chemical_formula_moiety         '2(C32 H30 Cl3 Cu2 N6 O), 2(F6 P), C H4 O'
_chemical_formula_sum            'C65 H64 Cl6 Cu4 F12 N12 O3 P2'
_chemical_formula_weight         1818.12

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'
O O 0.0106 0.0060 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   12.0536(5)
_cell_length_b                   24.9462(11)
_cell_length_c                   12.0840(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.631(2)
_cell_angle_gamma                90.00
_cell_volume                     3531.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4000
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      28.50

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1836
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6537
_exptl_absorpt_correction_T_max  0.7679
_exptl_absorpt_process_details   SADABS

_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       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            108528
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         0.82
_diffrn_reflns_theta_max         29.09
_reflns_number_total             9419
_reflns_number_gt                8101
_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    ?
_computing_publication_material  ?

_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)+(0.0439P)²+2.6246P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9419
_refine_ls_number_parameters     483
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0940
_refine_ls_wR_factor_gt          0.0808
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_restrained_S_all      1.137
_refine_ls_shift/su_max          0.003
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.860446(18) 0.036175(7) 0.901848(16) 0.01297(4) Uani 1 d . . .
Cu2 Cu 0.635533(17) 0.039444(7) 0.584290(16) 0.01238(4) Uani 1 d . . .
Cl2 Cl 0.95967(4) -0.022943(16) 0.81956(4) 0.01964(9) Uani 1 d . . .
Cl3 Cl 0.53512(4) -0.018583(16) 0.66792(3) 0.01864(9) Uani 1 d . . .
Cl1 Cl 0.74337(4) 0.301970(18) 0.74849(4) 0.02510(11) Uani 1 d . . .
O1 O 0.75278(10) 0.06735(5) 0.74292(9) 0.0140(3) Uani 1 d . . .
N4 N 0.70933(12) 0.09084(5) 0.48716(11) 0.0125(3) Uani 1 d . . .
N5 N 0.73673(13) -0.01405(6) 0.53446(12) 0.0159(3) Uani 1 d . . .
N6 N 0.52827(12) 0.10102(6) 0.57972(12) 0.0150(3) Uani 1 d . . .
N2 N 0.97344(13) 0.09566(6) 0.91499(12) 0.0151(3) Uani 1 d . . .
N1 N 0.78748(12) 0.08727(5) 1.00001(11) 0.0136(3) Uani 1 d . . .
N3 N 0.75630(12) -0.01713(6) 0.94831(12) 0.0146(3) Uani 1 d . . .
C1 C 0.75105(14) 0.12009(7) 0.74406(13) 0.0132(3) Uani 1 d . . .
C15 C 0.70636(15) -0.00005(7) 1.03000(14) 0.0167(4) Uani 1 d . . .
C6 C 0.78013(15) 0.14998(6) 0.65578(14) 0.0135(3) Uani 1 d . . .
C5 C 0.77929(15) 0.20564(7) 0.65776(15) 0.0160(4) Uani 1 d . . .
H5 H 0.8010 0.2255 0.5992 0.019 Uiso 1 calc R . .
C11 C 1.11392(19) 0.18415(8) 0.93899(17) 0.0271(5) Uani 1 d . . .
H11 H 1.1631 0.2144 0.9483 0.032 Uiso 1 calc R . .
C3 C 0.71617(16) 0.20373(7) 0.83342(15) 0.0178(4) Uani 1 d . . .
H3 H 0.6930 0.2224 0.8927 0.021 Uiso 1 calc R . .
C17 C 0.59938(17) -0.08138(8) 1.01916(18) 0.0269(5) Uani 1 d . . .
H17 H 0.5460 -0.1036 1.0439 0.032 Uiso 1 calc R . .
C10 C 1.03411(17) 0.17901(7) 1.00351(16) 0.0222(4) Uani 1 d . . .
H10 H 1.0276 0.2057 1.0577 0.027 Uiso 1 calc R . .
C2 C 0.71993(15) 0.14808(7) 0.83380(14) 0.0145(4) Uani 1 d . . .
C13 C 1.05059(16) 0.10086(7) 0.85181(15) 0.0189(4) Uani 1 d . . .
H13 H 1.0565 0.0734 0.7991 0.023 Uiso 1 calc R . .
C18 C 0.65057(17) -0.09870(7) 0.93413(17) 0.0229(4) Uani 1 d . . .
H18 H 0.6322 -0.1327 0.8993 0.028 Uiso 1 calc R . .
C19 C 0.72906(16) -0.06552(7) 0.90088(15) 0.0187(4) Uani 1 d . . .
H19 H 0.7646 -0.0773 0.8429 0.022 Uiso 1 calc R . .
C16 C 0.62691(17) -0.03121(8) 1.06779(17) 0.0232(4) Uani 1 d . . .
H16 H 0.5922 -0.0185 1.1256 0.028 Uiso 1 calc R . .
C4 C 0.74646(15) 0.23187(7) 0.74586(14) 0.0173(4) Uani 1 d . . .
C8 C 0.87531(15) 0.12665(7) 1.05660(14) 0.0165(4) Uani 1 d . . .
H8A H 0.9128 0.1137 1.1338 0.020 Uiso 1 calc R . .
H8B H 0.8382 0.1614 1.0646 0.020 Uiso 1 calc R . .
C7 C 0.68745(15) 0.11518(7) 0.92468(14) 0.0157(4) Uani 1 d . . .
H7A H 0.6304 0.0881 0.8885 0.019 Uiso 1 calc R . .
H7B H 0.6512 0.1387 0.9720 0.019 Uiso 1 calc R . .
C12 C 1.12159(17) 0.14483(8) 0.86084(17) 0.0246(4) Uani 1 d . . .
H12 H 1.1746 0.1480 0.8142 0.029 Uiso 1 calc R . .
C14 C 0.74710(16) 0.05318(7) 1.08323(14) 0.0180(4) Uani 1 d . . .
H14A H 0.6839 0.0714 1.1076 0.022 Uiso 1 calc R . .
H14B H 0.8101 0.0474 1.1513 0.022 Uiso 1 calc R . .
C9 C 0.96350(15) 0.13447(7) 0.98842(14) 0.0163(4) Uani 1 d . . .
C26 C 0.76163(17) -0.06333(7) 0.57777(16) 0.0202(4) Uani 1 d . . .
H26 H 0.7259 -0.0755 0.6354 0.024 Uiso 1 calc R . .
C22 C 0.78907(15) 0.00333(7) 0.45409(14) 0.0166(4) Uani 1 d . . .
C25 C 0.83706(17) -0.09718(8) 0.54202(18) 0.0257(5) Uani 1 d . . .
H25 H 0.8520 -0.1321 0.5736 0.031 Uiso 1 calc R . .
C24 C 0.89025(17) -0.07930(8) 0.45957(19) 0.0277(5) Uani 1 d . . .
H24 H 0.9424 -0.1018 0.4335 0.033 Uiso 1 calc R . .
C21 C 0.74923(16) 0.05733(7) 0.40309(14) 0.0166(4) Uani 1 d . . .
H21A H 0.8128 0.0756 0.3795 0.020 Uiso 1 calc R . .
H21B H 0.6862 0.0523 0.3346 0.020 Uiso 1 calc R . .
C20 C 0.81106(15) 0.11860(7) 0.56164(14) 0.0148(4) Uani 1 d . . .
H20A H 0.8693 0.0915 0.5950 0.018 Uiso 1 calc R . .
H20B H 0.8451 0.1431 0.5143 0.018 Uiso 1 calc R . .
C23 C 0.86687(17) -0.02807(8) 0.41513(17) 0.0233(4) Uani 1 d . . .
H23 H 0.9035 -0.0148 0.3591 0.028 Uiso 1 calc R . .
C27 C 0.62098(15) 0.13011(7) 0.43233(14) 0.0156(4) Uani 1 d . . .
H27A H 0.5800 0.1164 0.3569 0.019 Uiso 1 calc R . .
H27B H 0.6580 0.1644 0.4207 0.019 Uiso 1 calc R . .
C28 C 0.53742(15) 0.13956(7) 0.50496(14) 0.0159(4) Uani 1 d . . .
C30 C 0.39556(18) 0.19205(8) 0.56341(19) 0.0289(5) Uani 1 d . . .
H30 H 0.3491 0.2232 0.5569 0.035 Uiso 1 calc R . .
C31 C 0.38938(17) 0.15341(8) 0.64319(18) 0.0262(5) Uani 1 d . . .
H31 H 0.3404 0.1579 0.6937 0.031 Uiso 1 calc R . .
C29 C 0.46972(17) 0.18530(7) 0.49285(17) 0.0225(4) Uani 1 d . . .
H29 H 0.4743 0.2115 0.4370 0.027 Uiso 1 calc R . .
C32 C 0.45608(16) 0.10793(8) 0.64808(15) 0.0200(4) Uani 1 d . . .
H32 H 0.4507 0.0807 0.7015 0.024 Uiso 1 calc R . .
P1 P 0.59595(5) 0.22765(2) 0.15584(5) 0.03125(12) Uani 1 d . . .
F2 F 0.63911(13) 0.16616(6) 0.17767(12) 0.0453(4) Uani 1 d . . .
F6 F 0.68292(13) 0.23485(6) 0.07600(13) 0.0627(4) Uani 1 d . . .
F5 F 0.55473(14) 0.28843(5) 0.13375(12) 0.0450(4) Uani 1 d . . .
F3 F 0.51335(12) 0.21943(6) 0.23818(12) 0.0502(4) Uani 1 d . . .
F1 F 0.49926(15) 0.20869(6) 0.04922(13) 0.0540(5) Uani 1 d . . .
F4 F 0.69529(14) 0.24576(7) 0.26214(13) 0.0581(4) Uani 1 d . . .
O2 O 0.8749(3) 0.16692(13) 0.3201(2) 0.0364(8) Uani 0.50 d PD . .
H99 H 0.8109(9) 0.1800(10) 0.292(3) 0.051 Uiso 0.50 d PD . .
C33 C 0.9435(4) 0.20657(19) 0.3349(4) 0.0398(13) Uani 0.50 d P . .
H33A H 0.9000 0.2401 0.3262 0.055 Uiso 0.50 calc PR . .
H33B H 0.9898 0.2052 0.2783 0.055 Uiso 0.50 calc PR . .
H33C H 0.9936 0.2049 0.4115 0.055 Uiso 0.50 calc PR . .


_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
Cu1 N2 1.9951(15) . ?
Cu1 N3 1.9978(15) . ?
Cu1 N1 2.0728(14) . ?
Cu1 O1 2.1915(11) . ?
Cu1 Cl2 2.2704(5) . ?
Cu2 N5 1.9943(15) . ?
Cu2 N6 2.0001(15) . ?
Cu2 N4 2.0749(14) . ?
Cu2 O1 2.2089(11) . ?
Cu2 Cl3 2.2712(5) . ?
Cl1 C4 1.7495(18) . ?
O1 C1 1.316(2) . ?
N4 C21 1.481(2) . ?
N4 C27 1.483(2) . ?
N4 C20 1.508(2) . ?
N5 C26 1.342(2) . ?
N5 C22 1.348(2) . ?
N6 C28 1.342(2) . ?
N6 C32 1.345(2) . ?
N2 C9 1.338(2) . ?
N2 C13 1.341(2) . ?
N1 C14 1.484(2) . ?
N1 C8 1.487(2) . ?
N1 C7 1.500(2) . ?
N3 C15 1.341(2) . ?
N3 C19 1.344(2) . ?
C1 C6 1.412(2) . ?
C1 C2 1.413(2) . ?
C15 C16 1.391(3) . ?
C15 C14 1.506(2) . ?
C6 C5 1.389(2) . ?
C6 C20 1.499(2) . ?
C5 C4 1.384(3) . ?
C5 H5 0.9500 . ?
C11 C10 1.379(3) . ?
C11 C12 1.380(3) . ?
C11 H11 0.9500 . ?
C3 C4 1.388(3) . ?
C3 C2 1.389(2) . ?
C3 H3 0.9500 . ?
C17 C18 1.386(3) . ?
C17 C16 1.389(3) . ?
C17 H17 0.9500 . ?
C10 C9 1.385(2) . ?
C10 H10 0.9500 . ?
C2 C7 1.495(2) . ?
C13 C12 1.380(3) . ?
C13 H13 0.9500 . ?
C18 C19 1.386(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C16 H16 0.9500 . ?
C8 C9 1.503(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C12 H12 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C26 C25 1.382(3) . ?
C26 H26 0.9500 . ?
C22 C23 1.387(3) . ?
C22 C21 1.512(2) . ?
C25 C24 1.380(3) . ?
C25 H25 0.9500 . ?
C24 C23 1.389(3) . ?
C24 H24 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C23 H23 0.9500 . ?
C27 C28 1.502(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.390(2) . ?
C30 C31 1.378(3) . ?
C30 C29 1.383(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.384(3) . ?
C31 H31 0.9500 . ?
C29 H29 0.9500 . ?
C32 H32 0.9500 . ?
P1 F3 1.5782(15) . ?
P1 F1 1.5919(15) . ?
P1 F6 1.5933(15) . ?
P1 F5 1.5983(15) . ?
P1 F4 1.6010(15) . ?
P1 F2 1.6212(15) . ?
O2 C33 1.275(6) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 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
N2 Cu1 N3 159.24(6) . . ?
N2 Cu1 N1 82.58(6) . . ?
N3 Cu1 N1 82.47(6) . . ?
N2 Cu1 O1 93.32(5) . . ?
N3 Cu1 O1 101.59(5) . . ?
N1 Cu1 O1 92.28(5) . . ?
N2 Cu1 Cl2 95.61(5) . . ?
N3 Cu1 Cl2 96.98(4) . . ?
N1 Cu1 Cl2 171.26(4) . . ?
O1 Cu1 Cl2 96.37(3) . . ?
N5 Cu2 N6 160.55(6) . . ?
N5 Cu2 N4 82.44(6) . . ?
N6 Cu2 N4 82.55(6) . . ?
N5 Cu2 O1 99.27(5) . . ?
N6 Cu2 O1 93.39(5) . . ?
N4 Cu2 O1 91.39(5) . . ?
N5 Cu2 Cl3 97.81(5) . . ?
N6 Cu2 Cl3 95.33(5) . . ?
N4 Cu2 Cl3 171.91(4) . . ?
O1 Cu2 Cl3 96.54(3) . . ?
C1 O1 Cu1 110.68(9) . . ?
C1 O1 Cu2 108.41(9) . . ?
Cu1 O1 Cu2 140.74(6) . . ?
C21 N4 C27 112.43(12) . . ?
C21 N4 C20 108.60(13) . . ?
C27 N4 C20 111.14(13) . . ?
C21 N4 Cu2 106.92(10) . . ?
C27 N4 Cu2 107.60(10) . . ?
C20 N4 Cu2 110.06(10) . . ?
C26 N5 C22 118.41(16) . . ?
C26 N5 Cu2 126.28(13) . . ?
C22 N5 Cu2 115.19(11) . . ?
C28 N6 C32 119.31(15) . . ?
C28 N6 Cu2 114.44(12) . . ?
C32 N6 Cu2 126.11(12) . . ?
C9 N2 C13 119.35(15) . . ?
C9 N2 Cu1 115.15(12) . . ?
C13 N2 Cu1 125.34(12) . . ?
C14 N1 C8 112.24(13) . . ?
C14 N1 C7 109.40(14) . . ?
C8 N1 C7 110.83(13) . . ?
C14 N1 Cu1 106.66(10) . . ?
C8 N1 Cu1 108.50(11) . . ?
C7 N1 Cu1 109.09(10) . . ?
C15 N3 C19 119.50(16) . . ?
C15 N3 Cu1 114.60(11) . . ?
C19 N3 Cu1 125.79(13) . . ?
O1 C1 C6 120.85(15) . . ?
O1 C1 C2 120.66(15) . . ?
C6 C1 C2 118.49(15) . . ?
N3 C15 C16 121.82(16) . . ?
N3 C15 C14 115.88(15) . . ?
C16 C15 C14 122.19(16) . . ?
C5 C6 C1 120.73(16) . . ?
C5 C6 C20 122.65(16) . . ?
C1 C6 C20 116.63(14) . . ?
C4 C5 C6 119.37(16) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C10 C11 C12 119.28(18) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
C4 C3 C2 119.58(17) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C18 C17 C16 119.39(19) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C11 C10 C9 119.25(18) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C3 C2 C1 120.38(16) . . ?
C3 C2 C7 122.48(16) . . ?
C1 C2 C7 117.09(15) . . ?
N2 C13 C12 122.15(18) . . ?
N2 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
C17 C18 C19 118.82(18) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
N3 C19 C18 121.86(18) . . ?
N3 C19 H19 119.1 . . ?
C18 C19 H19 119.1 . . ?
C17 C16 C15 118.60(19) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C5 C4 C3 121.41(16) . . ?
C5 C4 Cl1 119.84(13) . . ?
C3 C4 Cl1 118.75(14) . . ?
N1 C8 C9 110.63(14) . . ?
N1 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C2 C7 N1 112.85(14) . . ?
C2 C7 H7A 109.0 . . ?
N1 C7 H7A 109.0 . . ?
C2 C7 H7B 109.0 . . ?
N1 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C13 C12 C11 118.62(19) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
N1 C14 C15 109.99(14) . . ?
N1 C14 H14A 109.7 . . ?
C15 C14 H14A 109.7 . . ?
N1 C14 H14B 109.7 . . ?
C15 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N2 C9 C10 121.31(17) . . ?
N2 C9 C8 117.07(15) . . ?
C10 C9 C8 121.59(16) . . ?
N5 C26 C25 122.73(18) . . ?
N5 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
N5 C22 C23 122.11(16) . . ?
N5 C22 C21 114.99(15) . . ?
C23 C22 C21 122.70(16) . . ?
C24 C25 C26 118.68(18) . . ?
C24 C25 H25 120.7 . . ?
C26 C25 H25 120.7 . . ?
C25 C24 C23 119.35(19) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
N4 C21 C22 110.29(13) . . ?
N4 C21 H21A 109.6 . . ?
C22 C21 H21A 109.6 . . ?
N4 C21 H21B 109.6 . . ?
C22 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C6 C20 N4 112.35(14) . . ?
C6 C20 H20A 109.1 . . ?
N4 C20 H20A 109.1 . . ?
C6 C20 H20B 109.1 . . ?
N4 C20 H20B 109.1 . . ?
H20A C20 H20B 107.9 . . ?
C22 C23 C24 118.70(19) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
N4 C27 C28 110.63(13) . . ?
N4 C27 H27A 109.5 . . ?
C28 C27 H27A 109.5 . . ?
N4 C27 H27B 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
N6 C28 C29 121.31(17) . . ?
N6 C28 C27 116.99(15) . . ?
C29 C28 C27 121.66(16) . . ?
C31 C30 C29 119.70(19) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C32 118.48(19) . . ?
C30 C31 H31 120.8 . . ?
C32 C31 H31 120.8 . . ?
C30 C29 C28 118.91(18) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
N6 C32 C31 122.18(18) . . ?
N6 C32 H32 118.9 . . ?
C31 C32 H32 118.9 . . ?
F3 P1 F1 91.22(9) . . ?
F3 P1 F6 177.91(9) . . ?
F1 P1 F6 90.24(9) . . ?
F3 P1 F5 90.64(9) . . ?
F1 P1 F5 90.41(8) . . ?
F6 P1 F5 90.85(9) . . ?
F3 P1 F4 89.68(9) . . ?
F1 P1 F4 178.63(10) . . ?
F6 P1 F4 88.83(9) . . ?
F5 P1 F4 90.60(8) . . ?
F3 P1 F2 90.02(8) . . ?
F1 P1 F2 89.78(8) . . ?
F6 P1 F2 88.49(8) . . ?
F5 P1 F2 179.31(9) . . ?
F4 P1 F2 89.19(8) . . ?
O2 C33 H33A 109.5 . . ?
O2 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O2 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        29.09
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.116
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_R2618
_database_code_depnum_ccdc_archive 'CCDC 1034094'
_audit_update_record             
;
2014-11-13 deposited with the CCDC.
2014-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Zn2(LClO-bdpa)Cl2]PF6.MeOH'
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H30 Cl3 N6 O Zn2, F6 P, C H4 O'
_chemical_formula_sum            'C33 H34 Cl3 F6 N6 O2 P Zn2'
_chemical_formula_weight         928.76

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   12.1205(4)
_cell_length_b                   24.9231(8)
_cell_length_c                   12.2116(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.081(2)
_cell_angle_gamma                90.00
_cell_volume                     3593.16(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4000
_cell_measurement_theta_min      2.00
_cell_measurement_theta_max      28.00

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1880
_exptl_absorpt_coefficient_mu    1.676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6697
_exptl_absorpt_correction_T_max  0.7871
_exptl_absorpt_process_details   SADABS

_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       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            122582
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         30.01
_reflns_number_total             10467
_reflns_number_gt                8814
_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    ?
_computing_publication_material  ?

_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)+(0.0403P)²+2.0893P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10467
_refine_ls_number_parameters     483
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0819
_refine_ls_wR_factor_gt          0.0715
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.103
_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
Zn1 Zn 0.095006(16) 0.538347(7) 0.138811(15) 0.01170(5) Uani 1 1 d . . .
Zn2 Zn 0.373691(16) 0.532230(7) 0.350138(15) 0.01200(5) Uani 1 1 d . . .
Cl3 Cl 0.29777(4) 0.470720(17) 0.45200(4) 0.01963(9) Uani 1 1 d . . .
Cl2 Cl 0.16910(4) 0.480581(17) 0.02729(3) 0.01864(9) Uani 1 1 d . . .
N6 N 0.44236(12) 0.47999(6) 0.25026(12) 0.0151(3) Uani 1 1 d . . .
N3 N 0.02791(12) 0.48407(6) 0.23515(11) 0.0137(3) Uani 1 1 d . . .
P1 P 0.35067(4) 0.26706(2) 0.90613(4) 0.02253(11) Uani 1 1 d . . .
F6 F 0.33158(12) 0.32802(5) 0.85834(12) 0.0384(3) Uani 1 1 d . . .
F2 F 0.26886(12) 0.27907(6) 0.98698(12) 0.0445(4) Uani 1 1 d . . .
F5 F 0.36938(11) 0.20712(5) 0.95163(12) 0.0346(3) Uani 1 1 d . . .
F1 F 0.24474(12) 0.24846(6) 0.80981(11) 0.0429(4) Uani 1 1 d . . .
F3 F 0.45646(12) 0.28701(6) 0.99935(13) 0.0464(4) Uani 1 1 d . . .
F4 F 0.43119(13) 0.25620(6) 0.82165(13) 0.0513(4) Uani 1 1 d . . .
O1 O 0.23706(9) 0.56633(5) 0.24889(9) 0.0121(2) Uani 1 1 d . . .
C1 C 0.24078(13) 0.62040(7) 0.25024(12) 0.0111(3) Uani 1 1 d . . .
C3 C 0.15767(14) 0.70562(6) 0.28286(14) 0.0133(3) Uani 1 1 d . . .
H3 H 0.1005 0.7257 0.3063 0.016 Uiso 1 1 calc R . .
C4 C 0.24507(14) 0.73171(7) 0.24839(13) 0.0136(3) Uani 1 1 d . . .
C6 C 0.32997(13) 0.64743(6) 0.21793(13) 0.0119(3) Uani 1 1 d . . .
C5 C 0.33070(14) 0.70333(7) 0.21575(14) 0.0137(3) Uani 1 1 d . . .
H5 H 0.3896 0.7219 0.1920 0.016 Uiso 1 1 calc R . .
C2 C 0.15451(13) 0.64981(6) 0.28277(13) 0.0117(3) Uani 1 1 d . . .
C7 C 0.05988(13) 0.61922(6) 0.31508(13) 0.0126(3) Uani 1 1 d . . .
H7A H 0.0923 0.5918 0.3719 0.015 Uiso 1 1 calc R . .
H7B H 0.0140 0.6442 0.3497 0.015 Uiso 1 1 calc R . .
C9 C -0.00013(14) 0.64226(7) 0.04493(13) 0.0133(3) Uani 1 1 d . . .
C12 C 0.13070(16) 0.65924(8) -0.10772(15) 0.0208(4) Uani 1 1 d . . .
H12 H 0.1787 0.6648 -0.1584 0.025 Uiso 1 1 calc R . .
C13 C 0.13892(15) 0.61301(7) -0.04361(14) 0.0168(3) Uani 1 1 d . . .
H13 H 0.1920 0.5863 -0.0526 0.020 Uiso 1 1 calc R . .
C8 C -0.06987(14) 0.63173(7) 0.13094(14) 0.0138(3) Uani 1 1 d . . .
H8A H -0.0809 0.6658 0.1687 0.017 Uiso 1 1 calc R . .
H8B H -0.1454 0.6181 0.0922 0.017 Uiso 1 1 calc R . .
C10 C -0.01572(16) 0.68876(7) -0.01948(15) 0.0188(3) Uani 1 1 d . . .
H10 H -0.0713 0.7143 -0.0109 0.023 Uiso 1 1 calc R . .
C11 C 0.05068(17) 0.69731(8) -0.09618(15) 0.0230(4) Uani 1 1 d . . .
H11 H 0.0416 0.7290 -0.1406 0.028 Uiso 1 1 calc R . .
C14 C -0.09727(14) 0.55801(7) 0.25564(14) 0.0149(3) Uani 1 1 d . . .
H14A H -0.1664 0.5542 0.1949 0.018 Uiso 1 1 calc R . .
H14B H -0.1190 0.5753 0.3206 0.018 Uiso 1 1 calc R . .
C15 C -0.04875(14) 0.50301(7) 0.28985(14) 0.0146(3) Uani 1 1 d . . .
C17 C -0.04857(18) 0.41972(8) 0.38714(16) 0.0252(4) Uani 1 1 d . . .
H17 H -0.0748 0.3976 0.4393 0.030 Uiso 1 1 calc R . .
C16 C -0.08754(17) 0.47199(8) 0.36782(15) 0.0211(4) Uani 1 1 d . . .
H16 H -0.1399 0.4863 0.4073 0.025 Uiso 1 1 calc R . .
C18 C 0.02884(17) 0.40017(7) 0.32966(15) 0.0227(4) Uani 1 1 d . . .
H18 H 0.0559 0.3644 0.3409 0.027 Uiso 1 1 calc R . .
C20 C 0.42152(13) 0.61472(7) 0.18481(13) 0.0129(3) Uani 1 1 d . . .
H20A H 0.3864 0.5878 0.1279 0.015 Uiso 1 1 calc R . .
H20B H 0.4695 0.6386 0.1503 0.015 Uiso 1 1 calc R . .
C23 C 0.50133(15) 0.67428(7) 0.53496(15) 0.0191(3) Uani 1 1 d . . .
H23 H 0.5556 0.7009 0.5282 0.023 Uiso 1 1 calc R . .
C22 C 0.48282(14) 0.63061(7) 0.46201(14) 0.0141(3) Uani 1 1 d . . .
C21 C 0.54794(14) 0.62493(7) 0.37116(14) 0.0146(3) Uani 1 1 d . . .
H21A H 0.5535 0.6604 0.3364 0.018 Uiso 1 1 calc R . .
H21B H 0.6258 0.6126 0.4052 0.018 Uiso 1 1 calc R . .
C26 C 0.35127(15) 0.59600(7) 0.55370(14) 0.0169(3) Uani 1 1 d . . .
H26 H 0.2998 0.5682 0.5610 0.020 Uiso 1 1 calc R . .
C25 C 0.36284(16) 0.63888(8) 0.62611(15) 0.0204(4) Uani 1 1 d . . .
H25 H 0.3188 0.6413 0.6811 0.024 Uiso 1 1 calc R . .
C24 C 0.44044(16) 0.67862(8) 0.61696(16) 0.0219(4) Uani 1 1 d . . .
H24 H 0.4514 0.7084 0.6667 0.026 Uiso 1 1 calc R . .
C28 C 0.52583(14) 0.49836(7) 0.20397(14) 0.0155(3) Uani 1 1 d . . .
C29 C 0.56721(17) 0.46804(7) 0.12663(15) 0.0213(4) Uani 1 1 d . . .
H29 H 0.6262 0.4815 0.0946 0.026 Uiso 1 1 calc R . .
C27 C 0.57661(14) 0.55206(7) 0.24564(15) 0.0162(3) Uani 1 1 d . . .
H27A H 0.6428 0.5463 0.3088 0.019 Uiso 1 1 calc R . .
H27B H 0.6034 0.5703 0.1845 0.019 Uiso 1 1 calc R . .
C31 C 0.43468(17) 0.39899(7) 0.14415(15) 0.0229(4) Uani 1 1 d . . .
H31 H 0.4015 0.3648 0.1244 0.027 Uiso 1 1 calc R . .
C30 C 0.52073(18) 0.41767(8) 0.09700(15) 0.0250(4) Uani 1 1 d . . .
H30 H 0.5480 0.3962 0.0446 0.030 Uiso 1 1 calc R . .
N2 N 0.07446(12) 0.60459(6) 0.03098(11) 0.0131(3) Uani 1 1 d . . .
N1 N -0.01505(11) 0.59234(5) 0.21617(11) 0.0119(2) Uani 1 1 d . . .
N5 N 0.41014(12) 0.59179(6) 0.47264(11) 0.0138(3) Uani 1 1 d . . .
N4 N 0.49389(11) 0.58668(6) 0.28337(11) 0.0127(3) Uani 1 1 d . . .
Cl1 Cl 0.24810(4) 0.801728(17) 0.24527(4) 0.01978(9) Uani 1 1 d . . .
C32 C 0.39789(15) 0.43136(7) 0.22097(15) 0.0187(3) Uani 1 1 d . . .
H32 H 0.3391 0.4187 0.2541 0.022 Uiso 1 1 calc R . .
C19 C 0.06620(15) 0.43368(7) 0.25545(14) 0.0177(3) Uani 1 1 d . . .
H19 H 0.1210 0.4206 0.2174 0.021 Uiso 1 1 calc R . .
C33 C 0.1809(2) 0.29419(13) 0.5509(2) 0.0524(7) Uani 1 1 d . . .
H33A H 0.2517 0.2935 0.5249 0.079 Uiso 1 1 calc R . .
H33B H 0.1174 0.3012 0.4871 0.079 Uiso 1 1 calc R . .
H33C H 0.1698 0.2595 0.5845 0.079 Uiso 1 1 calc R . .
O2 O 0.18655(16) 0.33469(8) 0.63123(16) 0.0448(4) Uani 1 1 d D . .
H2 H 0.2271(3) 0.3244(2) 0.6928(3) 0.067 Uiso 1 1 d 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
Zn1 O1 2.0518(11) . ?
Zn1 N3 2.0757(14) . ?
Zn1 N2 2.0913(14) . ?
Zn1 N1 2.2479(13) . ?
Zn1 Cl2 2.2995(4) . ?
Zn2 O1 2.0166(11) . ?
Zn2 N6 2.0821(14) . ?
Zn2 N5 2.0826(14) . ?
Zn2 N4 2.2730(14) . ?
Zn2 Cl3 2.2940(4) . ?
N6 C32 1.342(2) . ?
N6 C28 1.346(2) . ?
N3 C19 1.342(2) . ?
N3 C15 1.347(2) . ?
P1 F2 1.5782(13) . ?
P1 F3 1.5895(14) . ?
P1 F5 1.5921(14) . ?
P1 F4 1.5955(13) . ?
P1 F1 1.6010(14) . ?
P1 F6 1.6251(14) . ?
O1 C1 1.3482(19) . ?
C1 C6 1.404(2) . ?
C1 C2 1.406(2) . ?
C3 C4 1.387(2) . ?
C3 C2 1.391(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(2) . ?
C4 Cl1 1.7459(17) . ?
C6 C5 1.394(2) . ?
C6 C20 1.504(2) . ?
C5 H5 0.9500 . ?
C2 C7 1.502(2) . ?
C7 N1 1.495(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 N2 1.341(2) . ?
C9 C10 1.389(2) . ?
C9 C8 1.513(2) . ?
C12 C13 1.384(2) . ?
C12 C11 1.387(3) . ?
C12 H12 0.9500 . ?
C13 N2 1.344(2) . ?
C13 H13 0.9500 . ?
C8 N1 1.475(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 C11 1.383(3) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C14 N1 1.475(2) . ?
C14 C15 1.513(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.388(2) . ?
C17 C18 1.381(3) . ?
C17 C16 1.388(3) . ?
C17 H17 0.9500 . ?
C16 H16 0.9500 . ?
C18 C19 1.382(2) . ?
C18 H18 0.9500 . ?
C20 N4 1.493(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C23 C24 1.376(3) . ?
C23 C22 1.392(2) . ?
C23 H23 0.9500 . ?
C22 N5 1.334(2) . ?
C22 C21 1.507(2) . ?
C21 N4 1.473(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C26 N5 1.349(2) . ?
C26 C25 1.374(2) . ?
C26 H26 0.9500 . ?
C25 C24 1.388(3) . ?
C25 H25 0.9500 . ?
C24 H24 0.9500 . ?
C28 C29 1.389(2) . ?
C28 C27 1.512(2) . ?
C29 C30 1.390(3) . ?
C29 H29 0.9500 . ?
C27 N4 1.473(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C31 C30 1.381(3) . ?
C31 C32 1.385(2) . ?
C31 H31 0.9500 . ?
C30 H30 0.9500 . ?
C32 H32 0.9500 . ?
C19 H19 0.9500 . ?
C33 O2 1.398(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 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
O1 Zn1 N3 103.21(5) . . ?
O1 Zn1 N2 96.13(5) . . ?
N3 Zn1 N2 149.92(6) . . ?
O1 Zn1 N1 90.63(5) . . ?
N3 Zn1 N1 78.82(5) . . ?
N2 Zn1 N1 78.15(5) . . ?
O1 Zn1 Cl2 102.62(3) . . ?
N3 Zn1 Cl2 100.56(4) . . ?
N2 Zn1 Cl2 97.36(4) . . ?
N1 Zn1 Cl2 166.45(4) . . ?
O1 Zn2 N6 106.62(5) . . ?
O1 Zn2 N5 98.70(5) . . ?
N6 Zn2 N5 144.94(6) . . ?
O1 Zn2 N4 91.87(5) . . ?
N6 Zn2 N4 77.85(5) . . ?
N5 Zn2 N4 77.48(5) . . ?
O1 Zn2 Cl3 103.86(3) . . ?
N6 Zn2 Cl3 99.34(4) . . ?
N5 Zn2 Cl3 97.63(4) . . ?
N4 Zn2 Cl3 164.12(4) . . ?
C32 N6 C28 119.34(15) . . ?
C32 N6 Zn2 122.10(12) . . ?
C28 N6 Zn2 118.13(11) . . ?
C19 N3 C15 119.00(14) . . ?
C19 N3 Zn1 123.43(11) . . ?
C15 N3 Zn1 117.10(11) . . ?
F2 P1 F3 90.68(9) . . ?
F2 P1 F5 91.13(8) . . ?
F3 P1 F5 90.89(8) . . ?
F2 P1 F4 178.23(10) . . ?
F3 P1 F4 90.22(9) . . ?
F5 P1 F4 90.39(8) . . ?
F2 P1 F1 90.09(9) . . ?
F3 P1 F1 178.24(9) . . ?
F5 P1 F1 90.68(8) . . ?
F4 P1 F1 88.98(8) . . ?
F2 P1 F6 89.36(8) . . ?
F3 P1 F6 89.48(8) . . ?
F5 P1 F6 179.39(8) . . ?
F4 P1 F6 89.12(8) . . ?
F1 P1 F6 88.94(8) . . ?
C1 O1 Zn2 113.15(9) . . ?
C1 O1 Zn1 111.63(9) . . ?
Zn2 O1 Zn1 135.18(6) . . ?
O1 C1 C6 120.13(14) . . ?
O1 C1 C2 119.97(14) . . ?
C6 C1 C2 119.90(15) . . ?
C4 C3 C2 119.42(15) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C5 C4 C3 121.37(16) . . ?
C5 C4 Cl1 118.86(12) . . ?
C3 C4 Cl1 119.77(13) . . ?
C5 C6 C1 119.58(15) . . ?
C5 C6 C20 121.90(14) . . ?
C1 C6 C20 118.51(14) . . ?
C4 C5 C6 119.75(15) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C3 C2 C1 119.96(15) . . ?
C3 C2 C7 121.98(14) . . ?
C1 C2 C7 118.06(14) . . ?
N1 C7 C2 112.05(12) . . ?
N1 C7 H7A 109.2 . . ?
C2 C7 H7A 109.2 . . ?
N1 C7 H7B 109.2 . . ?
C2 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
N2 C9 C10 121.43(15) . . ?
N2 C9 C8 117.74(14) . . ?
C10 C9 C8 120.81(15) . . ?
C13 C12 C11 118.35(16) . . ?
C13 C12 H12 120.8 . . ?
C11 C12 H12 120.8 . . ?
N2 C13 C12 122.34(17) . . ?
N2 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
N1 C8 C9 111.86(13) . . ?
N1 C8 H8A 109.2 . . ?
C9 C8 H8A 109.2 . . ?
N1 C8 H8B 109.2 . . ?
C9 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C11 C10 C9 119.13(17) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C12 119.41(17) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
N1 C14 C15 111.52(13) . . ?
N1 C14 H14A 109.3 . . ?
C15 C14 H14A 109.3 . . ?
N1 C14 H14B 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
N3 C15 C16 121.59(16) . . ?
N3 C15 C14 116.71(14) . . ?
C16 C15 C14 121.53(15) . . ?
C18 C17 C16 119.27(17) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C16 C15 118.96(17) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C17 C18 C19 118.75(17) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
N4 C20 C6 111.82(12) . . ?
N4 C20 H20A 109.3 . . ?
C6 C20 H20A 109.3 . . ?
N4 C20 H20B 109.3 . . ?
C6 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
C24 C23 C22 119.47(17) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
N5 C22 C23 121.26(15) . . ?
N5 C22 C21 118.09(14) . . ?
C23 C22 C21 120.62(15) . . ?
N4 C21 C22 112.08(13) . . ?
N4 C21 H21A 109.2 . . ?
C22 C21 H21A 109.2 . . ?
N4 C21 H21B 109.2 . . ?
C22 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
N5 C26 C25 122.61(17) . . ?
N5 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
C26 C25 C24 118.40(16) . . ?
C26 C25 H25 120.8 . . ?
C24 C25 H25 120.8 . . ?
C23 C24 C25 119.17(17) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
N6 C28 C29 121.47(17) . . ?
N6 C28 C27 116.55(14) . . ?
C29 C28 C27 121.88(16) . . ?
C28 C29 C30 118.74(17) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 H29 120.6 . . ?
N4 C27 C28 111.68(13) . . ?
N4 C27 H27A 109.3 . . ?
C28 C27 H27A 109.3 . . ?
N4 C27 H27B 109.3 . . ?
C28 C27 H27B 109.3 . . ?
H27A C27 H27B 107.9 . . ?
C30 C31 C32 118.37(18) . . ?
C30 C31 H31 120.8 . . ?
C32 C31 H31 120.8 . . ?
C31 C30 C29 119.72(17) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C9 N2 C13 119.27(15) . . ?
C9 N2 Zn1 117.42(11) . . ?
C13 N2 Zn1 123.05(12) . . ?
C8 N1 C14 112.77(13) . . ?
C8 N1 C7 111.48(13) . . ?
C14 N1 C7 109.13(12) . . ?
C8 N1 Zn1 108.49(9) . . ?
C14 N1 Zn1 107.40(10) . . ?
C7 N1 Zn1 107.33(9) . . ?
C22 N5 C26 119.03(15) . . ?
C22 N5 Zn2 118.97(11) . . ?
C26 N5 Zn2 121.41(12) . . ?
C21 N4 C27 112.62(13) . . ?
C21 N4 C20 111.54(13) . . ?
C27 N4 C20 109.84(12) . . ?
C21 N4 Zn2 109.93(9) . . ?
C27 N4 Zn2 107.42(10) . . ?
C20 N4 Zn2 105.15(9) . . ?
N6 C32 C31 122.35(17) . . ?
N6 C32 H32 118.8 . . ?
C31 C32 H32 118.8 . . ?
N3 C19 C18 122.39(17) . . ?
N3 C19 H19 118.8 . . ?
C18 C19 H19 118.8 . . ?
O2 C33 H33A 109.5 . . ?
O2 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O2 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 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
C2 C3 C4 C5 -1.2(2) . . . . ?
C2 C3 C4 Cl1 178.60(12) . . . . ?
O1 C1 C6 C5 177.67(14) . . . . ?
C2 C1 C6 C5 -1.6(2) . . . . ?
O1 C1 C6 C20 -1.4(2) . . . . ?
C2 C1 C6 C20 179.35(14) . . . . ?
C3 C4 C5 C6 -0.4(2) . . . . ?
Cl1 C4 C5 C6 179.83(12) . . . . ?
C1 C6 C5 C4 1.7(2) . . . . ?
C20 C6 C5 C4 -179.21(15) . . . . ?
C4 C3 C2 C1 1.4(2) . . . . ?
C4 C3 C2 C7 -177.72(15) . . . . ?
O1 C1 C2 C3 -179.23(14) . . . . ?
C6 C1 C2 C3 0.0(2) . . . . ?
O1 C1 C2 C7 -0.1(2) . . . . ?
C6 C1 C2 C7 179.13(14) . . . . ?
C3 C2 C7 N1 109.40(17) . . . . ?
C1 C2 C7 N1 -69.70(18) . . . . ?
C11 C12 C13 N2 -1.8(3) . . . . ?
N2 C9 C8 N1 22.5(2) . . . . ?
C10 C9 C8 N1 -159.33(15) . . . . ?
N2 C9 C10 C11 -2.8(3) . . . . ?
C8 C9 C10 C11 179.14(16) . . . . ?
C9 C10 C11 C12 0.4(3) . . . . ?
C13 C12 C11 C10 1.8(3) . . . . ?
C19 N3 C15 C16 1.1(2) . . . . ?
C19 N3 C15 C14 -174.31(15) . . . . ?
N1 C14 C15 N3 -30.4(2) . . . . ?
N1 C14 C15 C16 154.23(16) . . . . ?
C18 C17 C16 C15 0.9(3) . . . . ?
N3 C15 C16 C17 -1.9(3) . . . . ?
C14 C15 C16 C17 173.25(17) . . . . ?
C16 C17 C18 C19 0.8(3) . . . . ?
C5 C6 C20 N4 110.97(17) . . . . ?
C1 C6 C20 N4 -69.98(18) . . . . ?
C24 C23 C22 N5 -2.5(3) . . . . ?
C24 C23 C22 C21 179.77(16) . . . . ?
N5 C22 C21 N4 19.6(2) . . . . ?
C23 C22 C21 N4 -162.62(15) . . . . ?
N5 C26 C25 C24 -1.7(3) . . . . ?
C22 C23 C24 C25 0.9(3) . . . . ?
C26 C25 C24 C23 1.1(3) . . . . ?
C32 N6 C28 C29 -0.1(3) . . . . ?
Zn2 N6 C28 C29 -172.77(13) . . . . ?
C32 N6 C28 C27 -176.62(15) . . . . ?
Zn2 N6 C28 C27 10.73(19) . . . . ?
N6 C28 C29 C30 0.0(3) . . . . ?
C27 C28 C29 C30 176.31(17) . . . . ?
N6 C28 C27 N4 -29.0(2) . . . . ?
C29 C28 C27 N4 154.48(16) . . . . ?
C32 C31 C30 C29 -0.5(3) . . . . ?
C28 C29 C30 C31 0.3(3) . . . . ?
C10 C9 N2 C13 2.8(2) . . . . ?
C8 C9 N2 C13 -179.06(14) . . . . ?
C12 C13 N2 C9 -0.5(2) . . . . ?
O1 Zn1 N2 C9 -97.78(12) . . . . ?
N3 Zn1 N2 C9 32.31(18) . . . . ?
N1 Zn1 N2 C9 -8.43(11) . . . . ?
Cl2 Zn1 N2 C9 158.60(11) . . . . ?
O1 Zn1 N2 C13 76.28(13) . . . . ?
N3 Zn1 N2 C13 -153.63(12) . . . . ?
N1 Zn1 N2 C13 165.63(14) . . . . ?
Cl2 Zn1 N2 C13 -27.34(13) . . . . ?
C9 C8 N1 C14 -145.89(14) . . . . ?
C9 C8 N1 C7 90.93(15) . . . . ?
C15 C14 N1 C8 149.74(14) . . . . ?
C15 C14 N1 C7 -85.79(16) . . . . ?
C2 C7 N1 C8 -61.48(17) . . . . ?
C2 C7 N1 C14 173.30(13) . . . . ?
C23 C22 N5 C26 2.0(2) . . . . ?
C21 C22 N5 C26 179.77(15) . . . . ?
C22 C21 N4 C27 -139.21(14) . . . . ?
C22 C21 N4 C20 96.76(15) . . . . ?
C28 C27 N4 C21 151.76(14) . . . . ?
C28 C27 N4 C20 -83.27(16) . . . . ?
C6 C20 N4 C21 -58.66(17) . . . . ?
C6 C20 N4 C27 175.76(13) . . . . ?
C28 N6 C32 C31 -0.1(3) . . . . ?
C30 C31 C32 N6 0.4(3) . . . . ?
C15 N3 C19 C18 0.8(3) . . . . ?
C17 C18 C19 N3 -1.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.099

