# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_rf2633a
_database_code_depnum_ccdc_archive 'CCDC 1444958'
_audit_update_record             
;
2015-12-31 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Ni2(LClO-bdpa)(mu2-OAc)2](PF6).3H2O'
_chemical_formula_moiety         'C36 H36 Cl N6 Ni2 O5, F6 P, 3(H2 O)'
_chemical_formula_sum            'C36 H42 Cl F6 N6 Ni2 O8 P'
_chemical_formula_weight         984.56

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'
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                   10.4453(3)
_cell_length_b                   20.6559(6)
_cell_length_c                   19.7889(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.2410(10)
_cell_angle_gamma                90.00
_cell_volume                     4156.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9907
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      29.84

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2024
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7568
_exptl_absorpt_correction_T_max  0.8620
_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       'φ and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            101401
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         30.09
_reflns_number_total             12155
_reflns_number_gt                9422
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0588P)²+4.0257P] 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         12155
_refine_ls_number_parameters     598
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.1243
_refine_ls_wR_factor_gt          0.1051
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.66478(3) 0.202820(12) 0.358728(15) 0.01227(7) Uani 1 1 d . . .
F1 F 0.5049(2) 0.04292(8) 0.73638(10) 0.0402(4) Uani 1 1 d . . .
Ni2 Ni 0.87015(3) 0.291472(12) 0.483810(15) 0.01181(7) Uani 1 1 d . . .
F2 F 0.6468(2) 0.17204(9) 0.70543(16) 0.0689(8) Uani 1 1 d . . .
Cl3 Cl 1.27179(6) 0.02531(3) 0.43862(4) 0.02436(13) Uani 1 1 d . . .
P1 P 0.57443(7) 0.10793(3) 0.72049(4) 0.02248(14) Uani 1 1 d . . .
O2 O 0.58329(16) 0.20750(8) 0.44389(9) 0.0176(3) Uani 1 1 d . . .
O3 O 0.68788(16) 0.29193(8) 0.50407(9) 0.0171(3) Uani 1 1 d . . .
O1 O 0.84485(15) 0.21309(7) 0.42098(8) 0.0136(3) Uani 1 1 d . . .
O4 O 0.63056(16) 0.29939(7) 0.33806(9) 0.0170(3) Uani 1 1 d . . .
O5 O 0.81099(16) 0.35070(7) 0.39870(9) 0.0173(3) Uani 1 1 d . . .
N4 N 1.07007(19) 0.29636(8) 0.48085(11) 0.0149(4) Uani 1 1 d . . .
N1 N 0.67721(18) 0.10062(8) 0.36501(10) 0.0128(3) Uani 1 1 d . . .
N3 N 0.75513(19) 0.18594(9) 0.27713(10) 0.0140(4) Uani 1 1 d . . .
N5 N 0.92571(19) 0.37641(9) 0.54001(10) 0.0163(4) Uani 1 1 d . . .
N6 N 0.94373(19) 0.22654(9) 0.56553(10) 0.0152(4) Uani 1 1 d . . .
N2 N 0.47739(19) 0.17642(9) 0.30301(11) 0.0168(4) Uani 1 1 d . . .
C6 C 1.0683(2) 0.19143(10) 0.42139(12) 0.0151(4) Uani 1 1 d . . .
C2 C 0.9149(2) 0.10313(10) 0.42459(12) 0.0138(4) Uani 1 1 d . . .
C1 C 0.9398(2) 0.17014(10) 0.42170(11) 0.0129(4) Uani 1 1 d . . .
C5 C 1.1694(2) 0.14656(11) 0.42584(12) 0.0164(4) Uani 1 1 d . . .
H5 H 1.2559 0.1608 0.4257 0.020 Uiso 1 1 calc R . .
C3 C 1.0176(2) 0.05933(10) 0.42928(12) 0.0160(4) Uani 1 1 d . . .
H3 H 1.0013 0.0142 0.4317 0.019 Uiso 1 1 calc R . .
C4 C 1.1433(2) 0.08102(11) 0.43042(13) 0.0174(4) Uani 1 1 d . . .
C9 C 0.4435(2) 0.11587(10) 0.31789(12) 0.0157(4) Uani 1 1 d . . .
C11 C 0.2361(2) 0.12507(13) 0.23733(15) 0.0260(5) Uani 1 1 d . . .
H11 H 0.1532 0.1076 0.2149 0.031 Uiso 1 1 calc R . .
C8 C 0.5446(2) 0.08043(10) 0.37171(12) 0.0155(4) Uani 1 1 d . . .
H8A H 0.5329 0.0909 0.4188 0.019 Uiso 1 1 calc R . .
H8B H 0.5340 0.0331 0.3646 0.019 Uiso 1 1 calc R . .
C12 C 0.2699(3) 0.18698(13) 0.22237(15) 0.0276(6) Uani 1 1 d . . .
H12 H 0.2107 0.2128 0.1896 0.033 Uiso 1 1 calc R . .
C13 C 0.3919(3) 0.21108(11) 0.25592(14) 0.0228(5) Uani 1 1 d . . .
H13 H 0.4156 0.2536 0.2452 0.027 Uiso 1 1 calc R . .
C10 C 0.3245(2) 0.08838(11) 0.28559(14) 0.0201(5) Uani 1 1 d . . .
H10 H 0.3036 0.0453 0.2961 0.024 Uiso 1 1 calc R . .
C7 C 0.7789(2) 0.08040(10) 0.42701(12) 0.0145(4) Uani 1 1 d . . .
H7A H 0.7791 0.0326 0.4304 0.017 Uiso 1 1 calc R . .
H7B H 0.7558 0.0980 0.4692 0.017 Uiso 1 1 calc R . .
C15 C 0.7710(2) 0.12324(10) 0.26275(12) 0.0138(4) Uani 1 1 d . . .
C14 C 0.7043(2) 0.07461(10) 0.30010(12) 0.0151(4) Uani 1 1 d . . .
H14A H 0.6204 0.0610 0.2689 0.018 Uiso 1 1 calc R . .
H14B H 0.7610 0.0358 0.3111 0.018 Uiso 1 1 calc R . .
C18 C 0.8842(2) 0.21600(11) 0.19688(13) 0.0177(4) Uani 1 1 d . . .
H18 H 0.9245 0.2490 0.1756 0.021 Uiso 1 1 calc R . .
C16 C 0.8404(2) 0.10439(10) 0.21402(12) 0.0167(4) Uani 1 1 d . . .
H16 H 0.8496 0.0598 0.2043 0.020 Uiso 1 1 calc R . .
C17 C 0.8957(2) 0.15113(11) 0.17998(13) 0.0178(4) Uani 1 1 d . . .
H17 H 0.9412 0.1393 0.1454 0.021 Uiso 1 1 calc R . .
C19 C 0.8127(2) 0.23110(11) 0.24525(12) 0.0170(4) Uani 1 1 d . . .
H19 H 0.8039 0.2753 0.2565 0.020 Uiso 1 1 calc R . .
C25 C 0.9124(3) 0.46207(12) 0.61947(14) 0.0241(5) Uani 1 1 d . . .
H25 H 0.8656 0.4825 0.6495 0.029 Uiso 1 1 calc R . .
C26 C 0.8640(2) 0.40612(11) 0.58358(13) 0.0200(5) Uani 1 1 d . . .
H26 H 0.7840 0.3883 0.5902 0.024 Uiso 1 1 calc R . .
C20 C 1.0942(2) 0.26280(10) 0.41823(12) 0.0159(4) Uani 1 1 d . . .
H20A H 1.1865 0.2698 0.4152 0.019 Uiso 1 1 calc R . .
H20B H 1.0361 0.2814 0.3760 0.019 Uiso 1 1 calc R . .
C21 C 1.0997(2) 0.36638(10) 0.47864(14) 0.0192(5) Uani 1 1 d . . .
H21A H 1.0633 0.3835 0.4314 0.023 Uiso 1 1 calc R . .
H21B H 1.1961 0.3732 0.4900 0.023 Uiso 1 1 calc R . .
C22 C 1.0392(2) 0.40157(10) 0.53065(13) 0.0174(4) Uani 1 1 d . . .
C23 C 1.0949(2) 0.45672(11) 0.56571(13) 0.0214(5) Uani 1 1 d . . .
H23 H 1.1761 0.4732 0.5591 0.026 Uiso 1 1 calc R . .
C24 C 1.0299(3) 0.48732(11) 0.61059(14) 0.0241(5) Uani 1 1 d . . .
H24 H 1.0658 0.5252 0.6349 0.029 Uiso 1 1 calc R . .
C30 C 1.0593(3) 0.11671(12) 0.63423(14) 0.0252(5) Uani 1 1 d . . .
H30 H 1.0986 0.0788 0.6571 0.030 Uiso 1 1 calc R . .
C29 C 1.1345(2) 0.16060(11) 0.60705(13) 0.0215(5) Uani 1 1 d . . .
H29 H 1.2258 0.1535 0.6112 0.026 Uiso 1 1 calc R . .
C32 C 0.8726(2) 0.18373(11) 0.59300(12) 0.0182(4) Uani 1 1 d . . .
H32 H 0.7814 0.1918 0.5882 0.022 Uiso 1 1 calc R . .
C27 C 1.1480(2) 0.26730(11) 0.54590(13) 0.0177(4) Uani 1 1 d . . .
H27A H 1.1729 0.3016 0.5814 0.021 Uiso 1 1 calc R . .
H27B H 1.2299 0.2486 0.5370 0.021 Uiso 1 1 calc R . .
C28 C 1.0730(2) 0.21527(11) 0.57351(12) 0.0163(4) Uani 1 1 d . . .
C31 C 0.9261(3) 0.12858(12) 0.62779(14) 0.0235(5) Uani 1 1 d . . .
H31 H 0.8732 0.0995 0.6468 0.028 Uiso 1 1 calc R . .
C35 C 0.7043(2) 0.34844(10) 0.35414(12) 0.0164(4) Uani 1 1 d . . .
C33 C 0.5979(2) 0.24960(11) 0.49029(12) 0.0164(4) Uani 1 1 d . . .
C36 C 0.6606(3) 0.41061(11) 0.31515(15) 0.0276(6) Uani 1 1 d . . .
H36A H 0.7200 0.4207 0.2848 0.041 Uiso 1 1 calc R . .
H36B H 0.6625 0.4460 0.3484 0.041 Uiso 1 1 calc R . .
H36C H 0.5709 0.4054 0.2870 0.041 Uiso 1 1 calc R . .
C34 C 0.4982(3) 0.25035(15) 0.53482(15) 0.0302(6) Uani 1 1 d . . .
H34A H 0.4436 0.2893 0.5245 0.045 Uiso 1 1 calc R . .
H34B H 0.5441 0.2505 0.5839 0.045 Uiso 1 1 calc R . .
H34C H 0.4424 0.2118 0.5249 0.045 Uiso 1 1 calc R . .
O6 O 0.3808(3) 0.33313(15) 0.37192(16) 0.0554(7) Uani 1 1 d D . .
H91 H 0.447(3) 0.321(3) 0.359(3) 0.083 Uiso 1 1 d D . .
H92 H 0.364(4) 0.300(2) 0.386(3) 0.083 Uiso 1 1 d D . .
O7 O 0.5678(5) 0.53607(19) 0.4263(3) 0.0981(14) Uani 1 1 d D . .
H93 H 0.563(4) 0.497(3) 0.435(4) 0.147 Uiso 1 1 d D . .
H94 H 0.539(4) 0.556(3) 0.455(4) 0.147 Uiso 1 1 d D . .
O8 O 0.5363(3) 0.40793(14) 0.47117(18) 0.0600(7) Uani 1 1 d D . .
H95 H 0.591(4) 0.380(2) 0.487(3) 0.090 Uiso 1 1 d D . .
H96 H 0.493(4) 0.390(3) 0.440(2) 0.090 Uiso 1 1 d D . .
F3A F 0.4559(7) 0.1304(3) 0.6610(3) 0.0565(16) Uani 0.622(14) 1 d P A 1
F4A F 0.6345(8) 0.0708(3) 0.6691(5) 0.081(3) Uani 0.622(14) 1 d P A 1
F5A F 0.6903(9) 0.0850(3) 0.7836(5) 0.098(4) Uani 0.622(14) 1 d P A 1
F6A F 0.5076(11) 0.1464(2) 0.7737(4) 0.077(3) Uani 0.622(14) 1 d P A 1
F3B F 0.5796(18) 0.0776(6) 0.6472(6) 0.089(5) Uani 0.378(14) 1 d P A 2
F4B F 0.7215(8) 0.0811(5) 0.7421(9) 0.075(4) Uani 0.378(14) 1 d P A 2
F5B F 0.5929(15) 0.1324(7) 0.7946(5) 0.081(4) Uani 0.378(14) 1 d P A 2
F6B F 0.4355(9) 0.1347(4) 0.6961(11) 0.084(5) Uani 0.378(14) 1 d P A 2


_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 O1 2.0097(16) . ?
Ni1 O4 2.0512(15) . ?
Ni1 O2 2.0569(17) . ?
Ni1 N3 2.0780(19) . ?
Ni1 N2 2.087(2) . ?
Ni1 N1 2.1169(18) . ?
F1 P1 1.5916(17) . ?
Ni2 O1 2.0216(15) . ?
Ni2 O3 2.0334(16) . ?
Ni2 O5 2.0586(16) . ?
Ni2 N5 2.0870(19) . ?
Ni2 N4 2.1049(19) . ?
Ni2 N6 2.106(2) . ?
F2 P1 1.586(2) . ?
Cl3 C4 1.747(2) . ?
P1 F4A 1.520(6) . ?
P1 F5B 1.521(8) . ?
P1 F6B 1.524(9) . ?
P1 F3A 1.570(6) . ?
P1 F3B 1.593(9) . ?
P1 F5A 1.599(4) . ?
P1 F4B 1.597(8) . ?
P1 F6A 1.601(5) . ?
O2 C33 1.248(3) . ?
O3 C33 1.267(3) . ?
O1 C1 1.328(3) . ?
O4 C35 1.268(3) . ?
O5 C35 1.254(3) . ?
N4 C21 1.482(3) . ?
N4 C27 1.483(3) . ?
N4 C20 1.491(3) . ?
N1 C14 1.478(3) . ?
N1 C8 1.482(3) . ?
N1 C7 1.487(3) . ?
N3 C19 1.343(3) . ?
N3 C15 1.345(3) . ?
N5 C26 1.338(3) . ?
N5 C22 1.345(3) . ?
N6 C28 1.344(3) . ?
N6 C32 1.347(3) . ?
N2 C13 1.341(3) . ?
N2 C9 1.350(3) . ?
C6 C5 1.393(3) . ?
C6 C1 1.413(3) . ?
C6 C20 1.503(3) . ?
C2 C3 1.390(3) . ?
C2 C1 1.412(3) . ?
C2 C7 1.507(3) . ?
C5 C4 1.388(3) . ?
C5 H5 0.9500 . ?
C3 C4 1.384(3) . ?
C3 H3 0.9500 . ?
C9 C10 1.383(3) . ?
C9 C8 1.507(3) . ?
C11 C12 1.377(4) . ?
C11 C10 1.391(4) . ?
C11 H11 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C12 C13 1.387(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C10 H10 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C15 C16 1.388(3) . ?
C15 C14 1.509(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C18 C19 1.377(3) . ?
C18 C17 1.393(3) . ?
C18 H18 0.9500 . ?
C16 C17 1.378(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C19 H19 0.9500 . ?
C25 C24 1.382(4) . ?
C25 C26 1.389(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.512(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.390(3) . ?
C23 C24 1.388(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C30 C29 1.386(4) . ?
C30 C31 1.390(4) . ?
C30 H30 0.9500 . ?
C29 C28 1.390(3) . ?
C29 H29 0.9500 . ?
C32 C31 1.381(3) . ?
C32 H32 0.9500 . ?
C27 C28 1.504(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C31 H31 0.9500 . ?
C35 C36 1.514(3) . ?
C33 C34 1.510(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 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
O1 Ni1 O4 96.63(6) . . ?
O1 Ni1 O2 89.86(7) . . ?
O4 Ni1 O2 91.82(7) . . ?
O1 Ni1 N3 88.06(7) . . ?
O4 Ni1 N3 95.60(7) . . ?
O2 Ni1 N3 172.48(7) . . ?
O1 Ni1 N2 169.82(7) . . ?
O4 Ni1 N2 92.82(7) . . ?
O2 Ni1 N2 86.05(7) . . ?
N3 Ni1 N2 94.79(8) . . ?
O1 Ni1 N1 91.89(6) . . ?
O4 Ni1 N1 170.77(7) . . ?
O2 Ni1 N1 91.72(7) . . ?
N3 Ni1 N1 81.12(7) . . ?
N2 Ni1 N1 78.93(7) . . ?
O1 Ni2 O3 97.39(6) . . ?
O1 Ni2 O5 90.02(6) . . ?
O3 Ni2 O5 92.26(7) . . ?
O1 Ni2 N5 169.17(7) . . ?
O3 Ni2 N5 92.85(7) . . ?
O5 Ni2 N5 86.05(7) . . ?
O1 Ni2 N4 90.69(7) . . ?
O3 Ni2 N4 170.03(7) . . ?
O5 Ni2 N4 93.59(7) . . ?
N5 Ni2 N4 79.51(7) . . ?
O1 Ni2 N6 86.30(7) . . ?
O3 Ni2 N6 92.58(7) . . ?
O5 Ni2 N6 174.26(7) . . ?
N5 Ni2 N6 96.79(8) . . ?
N4 Ni2 N6 82.07(7) . . ?
F4A P1 F3A 91.4(4) . . ?
F4A P1 F2 90.5(3) . . ?
F3A P1 F2 86.6(3) . . ?
F4A P1 F1 89.0(3) . . ?
F3A P1 F1 94.6(3) . . ?
F2 P1 F1 178.73(13) . . ?
F4A P1 F5A 91.0(4) . . ?
F3A P1 F5A 177.2(4) . . ?
F2 P1 F5A 95.0(3) . . ?
F1 P1 F5A 83.9(2) . . ?
F4A P1 F6A 178.6(4) . . ?
F3A P1 F6A 87.6(3) . . ?
F2 P1 F6A 90.4(3) . . ?
F1 P1 F6A 90.1(3) . . ?
F5A P1 F6A 90.0(4) . . ?
C33 O2 Ni1 129.18(15) . . ?
C33 O3 Ni2 129.54(15) . . ?
C1 O1 Ni1 121.87(13) . . ?
C1 O1 Ni2 122.42(14) . . ?
Ni1 O1 Ni2 115.70(7) . . ?
C35 O4 Ni1 131.20(15) . . ?
C35 O5 Ni2 127.24(15) . . ?
C21 N4 C27 110.11(18) . . ?
C21 N4 C20 110.68(18) . . ?
C27 N4 C20 111.70(17) . . ?
C21 N4 Ni2 105.24(14) . . ?
C27 N4 Ni2 107.89(14) . . ?
C20 N4 Ni2 110.99(14) . . ?
C14 N1 C8 110.15(17) . . ?
C14 N1 C7 111.83(17) . . ?
C8 N1 C7 110.68(17) . . ?
C14 N1 Ni1 109.44(13) . . ?
C8 N1 Ni1 103.89(13) . . ?
C7 N1 Ni1 110.56(13) . . ?
C19 N3 C15 118.7(2) . . ?
C19 N3 Ni1 125.49(15) . . ?
C15 N3 Ni1 115.21(15) . . ?
C26 N5 C22 118.7(2) . . ?
C26 N5 Ni2 127.80(16) . . ?
C22 N5 Ni2 113.44(15) . . ?
C28 N6 C32 118.1(2) . . ?
C28 N6 Ni2 112.38(15) . . ?
C32 N6 Ni2 126.15(16) . . ?
C13 N2 C9 118.7(2) . . ?
C13 N2 Ni1 128.51(16) . . ?
C9 N2 Ni1 112.80(15) . . ?
C5 C6 C1 119.99(19) . . ?
C5 C6 C20 120.9(2) . . ?
C1 C6 C20 119.06(19) . . ?
C3 C2 C1 119.6(2) . . ?
C3 C2 C7 120.90(19) . . ?
C1 C2 C7 119.39(19) . . ?
O1 C1 C2 120.71(19) . . ?
O1 C1 C6 119.97(18) . . ?
C2 C1 C6 119.30(19) . . ?
C4 C5 C6 119.7(2) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C4 C3 C2 120.4(2) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 121.0(2) . . ?
C3 C4 Cl3 119.64(17) . . ?
C5 C4 Cl3 119.38(18) . . ?
N2 C9 C10 122.2(2) . . ?
N2 C9 C8 115.36(19) . . ?
C10 C9 C8 122.5(2) . . ?
C12 C11 C10 119.4(2) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
N1 C8 C9 108.53(18) . . ?
N1 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
N1 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
C11 C12 C13 118.9(2) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
N2 C13 C12 122.3(2) . . ?
N2 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
C9 C10 C11 118.6(2) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
N1 C7 C2 112.75(17) . . ?
N1 C7 H7A 109.0 . . ?
C2 C7 H7A 109.0 . . ?
N1 C7 H7B 109.0 . . ?
C2 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
N3 C15 C16 121.8(2) . . ?
N3 C15 C14 116.39(19) . . ?
C16 C15 C14 121.79(19) . . ?
N1 C14 C15 112.67(17) . . ?
N1 C14 H14A 109.1 . . ?
C15 C14 H14A 109.1 . . ?
N1 C14 H14B 109.1 . . ?
C15 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
C19 C18 C17 118.4(2) . . ?
C19 C18 H18 120.8 . . ?
C17 C18 H18 120.8 . . ?
C17 C16 C15 119.2(2) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C16 C17 C18 119.2(2) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
N3 C19 C18 122.8(2) . . ?
N3 C19 H19 118.6 . . ?
C18 C19 H19 118.6 . . ?
C24 C25 C26 118.6(2) . . ?
C24 C25 H25 120.7 . . ?
C26 C25 H25 120.7 . . ?
N5 C26 C25 122.6(2) . . ?
N5 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
N4 C20 C6 110.81(18) . . ?
N4 C20 H20A 109.5 . . ?
C6 C20 H20A 109.5 . . ?
N4 C20 H20B 109.5 . . ?
C6 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
N4 C21 C22 109.05(19) . . ?
N4 C21 H21A 109.9 . . ?
C22 C21 H21A 109.9 . . ?
N4 C21 H21B 109.9 . . ?
C22 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
N5 C22 C23 122.0(2) . . ?
N5 C22 C21 115.28(19) . . ?
C23 C22 C21 122.7(2) . . ?
C24 C23 C22 118.8(2) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C25 C24 C23 119.3(2) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C29 C30 C31 119.6(2) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C30 C29 C28 118.4(2) . . ?
C30 C29 H29 120.8 . . ?
C28 C29 H29 120.8 . . ?
N6 C32 C31 123.0(2) . . ?
N6 C32 H32 118.5 . . ?
C31 C32 H32 118.5 . . ?
N4 C27 C28 112.12(18) . . ?
N4 C27 H27A 109.2 . . ?
C28 C27 H27A 109.2 . . ?
N4 C27 H27B 109.2 . . ?
C28 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
N6 C28 C29 122.6(2) . . ?
N6 C28 C27 115.2(2) . . ?
C29 C28 C27 122.1(2) . . ?
C32 C31 C30 118.3(2) . . ?
C32 C31 H31 120.9 . . ?
C30 C31 H31 120.9 . . ?
O5 C35 O4 126.7(2) . . ?
O5 C35 C36 116.3(2) . . ?
O4 C35 C36 117.0(2) . . ?
O2 C33 O3 126.7(2) . . ?
O2 C33 C34 116.9(2) . . ?
O3 C33 C34 116.4(2) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 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
C3 C2 C1 O1 -176.3(2) . . . . ?
C7 C2 C1 O1 -0.1(3) . . . . ?
C3 C2 C1 C6 2.0(3) . . . . ?
C7 C2 C1 C6 178.2(2) . . . . ?
C5 C6 C1 O1 176.6(2) . . . . ?
C20 C6 C1 O1 -1.7(3) . . . . ?
C5 C6 C1 C2 -1.8(3) . . . . ?
C20 C6 C1 C2 179.9(2) . . . . ?
C1 C6 C5 C4 0.1(4) . . . . ?
C20 C6 C5 C4 178.4(2) . . . . ?
C1 C2 C3 C4 -0.7(3) . . . . ?
C7 C2 C3 C4 -176.8(2) . . . . ?
C2 C3 C4 C5 -1.0(4) . . . . ?
C2 C3 C4 Cl3 178.34(18) . . . . ?
C6 C5 C4 C3 1.3(4) . . . . ?
C6 C5 C4 Cl3 -178.08(18) . . . . ?
C13 N2 C9 C10 0.8(4) . . . . ?
C13 N2 C9 C8 -179.5(2) . . . . ?
C14 N1 C8 C9 -70.0(2) . . . . ?
C7 N1 C8 C9 165.82(17) . . . . ?
N2 C9 C8 N1 -33.6(3) . . . . ?
C10 C9 C8 N1 146.1(2) . . . . ?
C10 C11 C12 C13 0.1(4) . . . . ?
C9 N2 C13 C12 0.3(4) . . . . ?
C11 C12 C13 N2 -0.8(4) . . . . ?
N2 C9 C10 C11 -1.4(4) . . . . ?
C8 C9 C10 C11 178.9(2) . . . . ?
C12 C11 C10 C9 0.9(4) . . . . ?
C14 N1 C7 C2 60.0(2) . . . . ?
C8 N1 C7 C2 -176.74(17) . . . . ?
C3 C2 C7 N1 -123.3(2) . . . . ?
C1 C2 C7 N1 60.6(3) . . . . ?
C19 N3 C15 C16 -2.7(3) . . . . ?
C19 N3 C15 C14 179.9(2) . . . . ?
C8 N1 C14 C15 138.09(19) . . . . ?
C7 N1 C14 C15 -98.4(2) . . . . ?
N3 C15 C14 N1 -22.6(3) . . . . ?
C16 C15 C14 N1 160.0(2) . . . . ?
N3 C15 C16 C17 0.7(3) . . . . ?
C14 C15 C16 C17 178.0(2) . . . . ?
C15 C16 C17 C18 2.0(3) . . . . ?
C19 C18 C17 C16 -2.6(4) . . . . ?
C15 N3 C19 C18 2.0(3) . . . . ?
C17 C18 C19 N3 0.7(4) . . . . ?
C22 N5 C26 C25 0.2(4) . . . . ?
C24 C25 C26 N5 -1.1(4) . . . . ?
C21 N4 C20 C6 178.23(19) . . . . ?
C27 N4 C20 C6 55.2(2) . . . . ?
C5 C6 C20 N4 -115.4(2) . . . . ?
C1 C6 C20 N4 62.9(3) . . . . ?
C27 N4 C21 C22 -71.9(2) . . . . ?
C20 N4 C21 C22 164.15(19) . . . . ?
C26 N5 C22 C23 1.1(4) . . . . ?
C26 N5 C22 C21 -177.9(2) . . . . ?
N4 C21 C22 N5 -32.9(3) . . . . ?
N4 C21 C22 C23 148.1(2) . . . . ?
N5 C22 C23 C24 -1.3(4) . . . . ?
C21 C22 C23 C24 177.6(2) . . . . ?
C26 C25 C24 C23 0.8(4) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
C31 C30 C29 C28 -0.5(4) . . . . ?
C28 N6 C32 C31 -1.1(3) . . . . ?
C21 N4 C27 C28 144.51(19) . . . . ?
C20 N4 C27 C28 -92.1(2) . . . . ?
C32 N6 C28 C29 1.9(3) . . . . ?
C32 N6 C28 C27 -175.9(2) . . . . ?
C30 C29 C28 N6 -1.1(4) . . . . ?
C30 C29 C28 C27 176.6(2) . . . . ?
N4 C27 C28 N6 -36.9(3) . . . . ?
N4 C27 C28 C29 145.2(2) . . . . ?
N6 C32 C31 C30 -0.4(4) . . . . ?
C29 C30 C31 C32 1.2(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        30.09
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.172
####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_R2678
_database_code_depnum_ccdc_archive 'CCDC 1444959'
_audit_update_record             
;
2015-12-31 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Ni2(L-Cl-O-bdpa)(mu-acetato)2]ClO4.CH3COCH3'
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H36 Cl N6 Ni2 O5, Cl O4, C3 H6 O'
_chemical_formula_sum            'C39 H42 Cl2 N6 Ni2 O10'
_chemical_formula_weight         943.09

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/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   10.1039(2)
_cell_length_b                   14.0417(2)
_cell_length_c                   28.0477(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.8950(10)
_cell_angle_gamma                90.00
_cell_volume                     3977.12(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9919
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      29.85

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1952
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7032
_exptl_absorpt_correction_T_max  0.8114
_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       'φ and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            76473
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         30.04
_reflns_number_total             11605
_reflns_number_gt                9342
_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)+(0.0526P)²+0.6038P] 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         11605
_refine_ls_number_parameters     536
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0995
_refine_ls_wR_factor_gt          0.0831
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.002
_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 0.24780(2) 0.605400(15) 0.114838(7) 0.00873(6) Uani 1 1 d . . .
Ni2 Ni 0.55897(2) 0.690234(15) 0.093240(8) 0.00897(6) Uani 1 1 d . . .
Cl1 Cl 0.46527(5) 0.81869(3) 0.335022(16) 0.01812(10) Uani 1 1 d . . .
Cl2 Cl 0.87437(4) 0.10380(3) 0.145047(15) 0.01406(9) Uani 1 1 d . . .
O3 O 0.54401(11) 0.55862(9) 0.06472(4) 0.0120(2) Uani 1 1 d . . .
O4 O 0.23926(12) 0.66799(9) 0.05014(4) 0.0135(3) Uani 1 1 d . . .
O2 O 0.35834(11) 0.49256(9) 0.09276(4) 0.0127(2) Uani 1 1 d . . .
O1 O 0.41295(11) 0.67233(9) 0.13989(4) 0.0106(2) Uani 1 1 d . . .
O5 O 0.42719(11) 0.75378(9) 0.04635(4) 0.0124(2) Uani 1 1 d . . .
O6 O 0.80633(15) 0.03017(10) 0.17048(5) 0.0252(3) Uani 1 1 d . . .
O7 O 0.78509(15) 0.18096(10) 0.13496(6) 0.0289(4) Uani 1 1 d . . .
O9 O 0.92243(15) 0.06618(11) 0.10111(5) 0.0285(3) Uani 1 1 d . . .
O8 O 0.98439(15) 0.13760(12) 0.17440(6) 0.0315(4) Uani 1 1 d . . .
N6 N 0.68964(13) 0.64008(11) 0.14835(5) 0.0117(3) Uani 1 1 d . . .
N2 N 0.08465(13) 0.51598(10) 0.10178(5) 0.0111(3) Uani 1 1 d . . .
N5 N 0.70274(14) 0.73671(11) 0.04697(5) 0.0129(3) Uani 1 1 d . . .
N1 N 0.22147(13) 0.54539(10) 0.18362(5) 0.0091(3) Uani 1 1 d . . .
N4 N 0.61201(14) 0.82261(10) 0.12527(5) 0.0121(3) Uani 1 1 d . . .
C19 C 0.13009(17) 0.80641(13) 0.12838(7) 0.0159(4) Uani 1 1 d . . .
H19 H 0.1498 0.8175 0.0960 0.019 Uiso 1 1 calc R . .
C14 C 0.11519(16) 0.59911(12) 0.20707(6) 0.0118(3) Uani 1 1 d . . .
H14A H 0.1297 0.5960 0.2421 0.014 Uiso 1 1 calc R . .
H14B H 0.0285 0.5693 0.1990 0.014 Uiso 1 1 calc R . .
C3 C 0.40447(16) 0.68219(12) 0.26932(6) 0.0118(3) Uani 1 1 d . . .
H3 H 0.3847 0.6424 0.2956 0.014 Uiso 1 1 calc R . .
C6 C 0.46387(16) 0.80061(12) 0.19265(6) 0.0110(3) Uani 1 1 d . . .
C1 C 0.42269(16) 0.70585(12) 0.18391(6) 0.0105(3) Uani 1 1 d . . .
C13 C -0.00409(16) 0.51915(13) 0.06511(6) 0.0139(3) Uani 1 1 d . . .
H13 H 0.0026 0.5687 0.0423 0.017 Uiso 1 1 calc R . .
C10 C -0.02273(17) 0.37668(13) 0.13063(6) 0.0135(3) Uani 1 1 d . . .
H10 H -0.0275 0.3279 0.1540 0.016 Uiso 1 1 calc R . .
C8 C 0.17950(16) 0.44618(12) 0.17387(6) 0.0112(3) Uani 1 1 d . . .
H8A H 0.1431 0.4178 0.2030 0.013 Uiso 1 1 calc R . .
H8B H 0.2567 0.4077 0.1647 0.013 Uiso 1 1 calc R . .
C16 C 0.07832(17) 0.77541(13) 0.22203(7) 0.0153(4) Uani 1 1 d . . .
H16 H 0.0627 0.7632 0.2547 0.018 Uiso 1 1 calc R . .
C4 C 0.44633(17) 0.77495(13) 0.27697(6) 0.0134(3) Uani 1 1 d . . .
C11 C -0.11403(17) 0.38031(13) 0.09253(7) 0.0155(4) Uani 1 1 d . . .
H11 H -0.1818 0.3336 0.0893 0.019 Uiso 1 1 calc R . .
C9 C 0.07519(16) 0.44540(12) 0.13394(6) 0.0108(3) Uani 1 1 d . . .
C7 C 0.34625(16) 0.54737(12) 0.21307(6) 0.0107(3) Uani 1 1 d . . .
H7A H 0.4161 0.5127 0.1962 0.013 Uiso 1 1 calc R . .
H7B H 0.3323 0.5143 0.2437 0.013 Uiso 1 1 calc R . .
C18 C 0.09324(18) 0.88272(13) 0.15613(7) 0.0186(4) Uani 1 1 d . . .
H18 H 0.0857 0.9448 0.1428 0.022 Uiso 1 1 calc R . .
C5 C 0.47492(17) 0.83418(13) 0.23902(6) 0.0132(3) Uani 1 1 d . . .
H5 H 0.5022 0.8980 0.2449 0.016 Uiso 1 1 calc R . .
C15 C 0.11264(16) 0.70178(13) 0.19142(6) 0.0125(3) Uani 1 1 d . . .
C12 C -0.10524(17) 0.45275(13) 0.05930(7) 0.0160(4) Uani 1 1 d . . .
H12 H -0.1670 0.4569 0.0331 0.019 Uiso 1 1 calc R . .
C17 C 0.06761(18) 0.86694(14) 0.20369(7) 0.0189(4) Uani 1 1 d . . .
H17 H 0.0429 0.9183 0.2236 0.023 Uiso 1 1 calc R . .
C2 C 0.39149(15) 0.64757(12) 0.22293(6) 0.0103(3) Uani 1 1 d . . .
C29 C 0.77141(17) 0.68908(14) 0.22548(7) 0.0153(4) Uani 1 1 d . . .
H29 H 0.7966 0.7392 0.2466 0.018 Uiso 1 1 calc R . .
C28 C 0.72894(16) 0.70899(13) 0.17887(6) 0.0122(3) Uani 1 1 d . . .
C27 C 0.72880(17) 0.80789(13) 0.15817(7) 0.0144(4) Uani 1 1 d . . .
H27A H 0.7270 0.8552 0.1843 0.017 Uiso 1 1 calc R . .
H27B H 0.8110 0.8179 0.1406 0.017 Uiso 1 1 calc R . .
C26 C 0.76366(17) 0.68606(14) 0.01380(7) 0.0162(4) Uani 1 1 d . . .
H26 H 0.7468 0.6196 0.0116 0.019 Uiso 1 1 calc R . .
C24 C 0.87787(18) 0.82311(15) -0.01372(8) 0.0230(4) Uani 1 1 d . . .
H24 H 0.9378 0.8525 -0.0346 0.028 Uiso 1 1 calc R . .
C30 C 0.77661(17) 0.59510(14) 0.24076(7) 0.0171(4) Uani 1 1 d . . .
H30 H 0.8054 0.5798 0.2724 0.020 Uiso 1 1 calc R . .
C20 C 0.49816(17) 0.86268(12) 0.15102(6) 0.0122(3) Uani 1 1 d . . .
H20A H 0.4203 0.8679 0.1288 0.015 Uiso 1 1 calc R . .
H20B H 0.5208 0.9274 0.1626 0.015 Uiso 1 1 calc R . .
C21 C 0.64614(17) 0.88502(13) 0.08508(6) 0.0142(4) Uani 1 1 d . . .
H21A H 0.6970 0.9407 0.0973 0.017 Uiso 1 1 calc R . .
H21B H 0.5640 0.9086 0.0689 0.017 Uiso 1 1 calc R . .
C31 C 0.73884(17) 0.52387(14) 0.20877(7) 0.0157(4) Uani 1 1 d . . .
H31 H 0.7429 0.4588 0.2180 0.019 Uiso 1 1 calc R . .
C32 C 0.69521(16) 0.54911(13) 0.16326(6) 0.0134(3) Uani 1 1 d . . .
H32 H 0.6681 0.5002 0.1417 0.016 Uiso 1 1 calc R . .
C22 C 0.72739(17) 0.83085(13) 0.05007(7) 0.0145(4) Uani 1 1 d . . .
C25 C 0.85061(19) 0.72686(15) -0.01759(7) 0.0224(4) Uani 1 1 d . . .
H25 H 0.8907 0.6893 -0.0413 0.027 Uiso 1 1 calc R . .
C23 C 0.81664(18) 0.87617(14) 0.02095(7) 0.0191(4) Uani 1 1 d . . .
H23 H 0.8353 0.9421 0.0247 0.023 Uiso 1 1 calc R . .
C33 C 0.46639(16) 0.48967(12) 0.07173(6) 0.0107(3) Uani 1 1 d . . .
C36 C 0.24688(18) 0.79608(14) -0.00488(7) 0.0179(4) Uani 1 1 d . . .
H36A H 0.2493 0.8627 0.0055 0.027 Uiso 1 1 calc R . .
H36B H 0.1547 0.7764 -0.0108 0.027 Uiso 1 1 calc R . .
H36C H 0.2957 0.7893 -0.0343 0.027 Uiso 1 1 calc R . .
C35 C 0.31008(16) 0.73385(12) 0.03374(6) 0.0110(3) Uani 1 1 d . . .
C34 C 0.50968(18) 0.39436(12) 0.05245(6) 0.0136(3) Uani 1 1 d . . .
H34A H 0.4494 0.3445 0.0630 0.020 Uiso 1 1 calc R . .
H34B H 0.5999 0.3803 0.0643 0.020 Uiso 1 1 calc R . .
H34C H 0.5078 0.3965 0.0175 0.020 Uiso 1 1 calc R . .
N3 N 0.13906(13) 0.71699(11) 0.14553(5) 0.0117(3) Uani 1 1 d . . .
C37 C 0.6492(2) 0.57165(16) 0.41509(8) 0.0247(4) Uani 1 1 d . . .
C38 C 0.7056(2) 0.6310(2) 0.37608(9) 0.0411(6) Uani 1 1 d . . .
H38A H 0.7964 0.6103 0.3704 0.062 Uiso 1 1 calc R . .
H38B H 0.7062 0.6982 0.3856 0.062 Uiso 1 1 calc R . .
H38C H 0.6512 0.6233 0.3468 0.062 Uiso 1 1 calc R . .
O10 O 0.69605(16) 0.49512(11) 0.42616(7) 0.0375(4) Uani 1 1 d . . .
C39 C 0.5323(2) 0.61229(15) 0.43901(8) 0.0270(5) Uani 1 1 d . . .
H39A H 0.4977 0.5653 0.4612 0.040 Uiso 1 1 calc R . .
H39B H 0.4634 0.6284 0.4149 0.040 Uiso 1 1 calc R . .
H39C H 0.5590 0.6699 0.4566 0.040 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 O4 2.0157(12) . ?
Ni1 O1 2.0209(12) . ?
Ni1 O2 2.0463(12) . ?
Ni1 N2 2.0948(14) . ?
Ni1 N3 2.1133(15) . ?
Ni1 N1 2.1297(14) . ?
Ni2 O3 2.0174(12) . ?
Ni2 O1 2.0198(12) . ?
Ni2 O5 2.0453(12) . ?
Ni2 N5 2.0845(15) . ?
Ni2 N6 2.1198(14) . ?
Ni2 N4 2.1254(15) . ?
Cl1 C4 1.7447(17) . ?
Cl2 O7 1.4321(14) . ?
Cl2 O9 1.4397(14) . ?
Cl2 O8 1.4417(15) . ?
Cl2 O6 1.4432(14) . ?
O3 C33 1.265(2) . ?
O4 C35 1.265(2) . ?
O2 C33 1.258(2) . ?
O1 C1 1.322(2) . ?
O5 C35 1.255(2) . ?
N6 C28 1.343(2) . ?
N6 C32 1.345(2) . ?
N2 C13 1.343(2) . ?
N2 C9 1.346(2) . ?
N5 C26 1.337(2) . ?
N5 C22 1.347(2) . ?
N1 C8 1.479(2) . ?
N1 C14 1.484(2) . ?
N1 C7 1.485(2) . ?
N4 C21 1.478(2) . ?
N4 C27 1.488(2) . ?
N4 C20 1.489(2) . ?
C19 N3 1.346(2) . ?
C19 C18 1.383(3) . ?
C19 H19 0.9500 . ?
C14 C15 1.507(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C3 C4 1.384(3) . ?
C3 C2 1.391(2) . ?
C3 H3 0.9500 . ?
C6 C5 1.385(2) . ?
C6 C1 1.413(2) . ?
C6 C20 1.506(2) . ?
C1 C2 1.410(2) . ?
C13 C12 1.389(2) . ?
C13 H13 0.9500 . ?
C10 C9 1.383(2) . ?
C10 C11 1.389(3) . ?
C10 H10 0.9500 . ?
C8 C9 1.512(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C16 C17 1.387(3) . ?
C16 C15 1.395(2) . ?
C16 H16 0.9500 . ?
C4 C5 1.389(3) . ?
C11 C12 1.384(3) . ?
C11 H11 0.9500 . ?
C7 C2 1.502(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C18 C17 1.385(3) . ?
C18 H18 0.9500 . ?
C5 H5 0.9500 . ?
C15 N3 1.340(2) . ?
C12 H12 0.9500 . ?
C17 H17 0.9500 . ?
C29 C30 1.388(3) . ?
C29 C28 1.391(2) . ?
C29 H29 0.9500 . ?
C28 C27 1.505(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C26 C25 1.388(3) . ?
C26 H26 0.9500 . ?
C24 C25 1.383(3) . ?
C24 C23 1.387(3) . ?
C24 H24 0.9500 . ?
C30 C31 1.389(3) . ?
C30 H30 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.507(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C31 C32 1.383(2) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C22 C23 1.391(3) . ?
C25 H25 0.9500 . ?
C23 H23 0.9500 . ?
C33 C34 1.514(2) . ?
C36 C35 1.516(2) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C37 O10 1.210(3) . ?
C37 C39 1.491(3) . ?
C37 C38 1.503(3) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
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
O4 Ni1 O1 96.92(5) . . ?
O4 Ni1 O2 94.17(5) . . ?
O1 Ni1 O2 90.72(5) . . ?
O4 Ni1 N2 95.39(5) . . ?
O1 Ni1 N2 167.29(5) . . ?
O2 Ni1 N2 85.25(5) . . ?
O4 Ni1 N3 92.07(5) . . ?
O1 Ni1 N3 87.02(5) . . ?
O2 Ni1 N3 173.58(5) . . ?
N2 Ni1 N3 95.68(5) . . ?
O4 Ni1 N1 170.09(5) . . ?
O1 Ni1 N1 89.74(5) . . ?
O2 Ni1 N1 93.07(5) . . ?
N2 Ni1 N1 78.47(5) . . ?
N3 Ni1 N1 80.92(6) . . ?
O3 Ni2 O1 95.51(5) . . ?
O3 Ni2 O5 96.09(5) . . ?
O1 Ni2 O5 89.82(5) . . ?
O3 Ni2 N5 94.85(5) . . ?
O1 Ni2 N5 168.90(5) . . ?
O5 Ni2 N5 85.14(5) . . ?
O3 Ni2 N6 91.23(5) . . ?
O1 Ni2 N6 86.38(5) . . ?
O5 Ni2 N6 172.06(5) . . ?
N5 Ni2 N6 97.36(5) . . ?
O3 Ni2 N4 169.50(5) . . ?
O1 Ni2 N4 90.83(5) . . ?
O5 Ni2 N4 92.29(5) . . ?
N5 Ni2 N4 79.53(6) . . ?
N6 Ni2 N4 80.80(6) . . ?
O7 Cl2 O9 109.67(10) . . ?
O7 Cl2 O8 109.42(10) . . ?
O9 Cl2 O8 109.51(9) . . ?
O7 Cl2 O6 109.42(9) . . ?
O9 Cl2 O6 109.87(9) . . ?
O8 Cl2 O6 108.94(9) . . ?
C33 O3 Ni2 132.69(11) . . ?
C35 O4 Ni1 129.65(11) . . ?
C33 O2 Ni1 131.10(11) . . ?
C1 O1 Ni2 121.82(10) . . ?
C1 O1 Ni1 121.70(10) . . ?
Ni2 O1 Ni1 116.43(6) . . ?
C35 O5 Ni2 132.18(11) . . ?
C28 N6 C32 118.54(15) . . ?
C28 N6 Ni2 112.90(12) . . ?
C32 N6 Ni2 124.13(11) . . ?
C13 N2 C9 118.52(15) . . ?
C13 N2 Ni1 128.00(12) . . ?
C9 N2 Ni1 113.41(11) . . ?
C26 N5 C22 118.57(16) . . ?
C26 N5 Ni2 127.80(13) . . ?
C22 N5 Ni2 113.46(12) . . ?
C8 N1 C14 110.70(13) . . ?
C8 N1 C7 110.70(13) . . ?
C14 N1 C7 110.96(13) . . ?
C8 N1 Ni1 104.41(10) . . ?
C14 N1 Ni1 108.32(10) . . ?
C7 N1 Ni1 111.56(10) . . ?
C21 N4 C27 110.80(13) . . ?
C21 N4 C20 110.46(13) . . ?
C27 N4 C20 111.17(14) . . ?
C21 N4 Ni2 104.96(11) . . ?
C27 N4 Ni2 108.93(11) . . ?
C20 N4 Ni2 110.34(10) . . ?
N3 C19 C18 122.54(17) . . ?
N3 C19 H19 118.7 . . ?
C18 C19 H19 118.7 . . ?
N1 C14 C15 111.28(14) . . ?
N1 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
N1 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C4 C3 C2 119.53(16) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C5 C6 C1 119.84(16) . . ?
C5 C6 C20 121.17(16) . . ?
C1 C6 C20 118.97(15) . . ?
O1 C1 C2 120.43(15) . . ?
O1 C1 C6 120.63(16) . . ?
C2 C1 C6 118.94(16) . . ?
N2 C13 C12 122.52(17) . . ?
N2 C13 H13 118.7 . . ?
C12 C13 H13 118.7 . . ?
C9 C10 C11 118.78(17) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
N1 C8 C9 109.40(14) . . ?
N1 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
N1 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
C17 C16 C15 118.45(18) . . ?
C17 C16 H16 120.8 . . ?
C15 C16 H16 120.8 . . ?
C3 C4 C5 120.99(16) . . ?
C3 C4 Cl1 119.98(14) . . ?
C5 C4 Cl1 119.03(14) . . ?
C12 C11 C10 119.28(16) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
N2 C9 C10 122.37(16) . . ?
N2 C9 C8 115.33(14) . . ?
C10 C9 C8 122.30(16) . . ?
N1 C7 C2 111.57(13) . . ?
N1 C7 H7A 109.3 . . ?
C2 C7 H7A 109.3 . . ?
N1 C7 H7B 109.3 . . ?
C2 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C19 C18 C17 118.71(18) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C6 C5 C4 120.25(16) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
N3 C15 C16 122.30(17) . . ?
N3 C15 C14 115.47(15) . . ?
C16 C15 C14 122.14(16) . . ?
C11 C12 C13 118.53(16) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C18 C17 C16 119.38(18) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C3 C2 C1 120.42(16) . . ?
C3 C2 C7 121.21(15) . . ?
C1 C2 C7 118.36(15) . . ?
C30 C29 C28 119.26(17) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
N6 C28 C29 121.99(17) . . ?
N6 C28 C27 114.99(15) . . ?
C29 C28 C27 122.98(16) . . ?
N4 C27 C28 110.97(14) . . ?
N4 C27 H27A 109.4 . . ?
C28 C27 H27A 109.4 . . ?
N4 C27 H27B 109.4 . . ?
C28 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
N5 C26 C25 122.50(19) . . ?
N5 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
C25 C24 C23 119.20(18) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C29 C30 C31 118.59(17) . . ?
C29 C30 H30 120.7 . . ?
C31 C30 H30 120.7 . . ?
N4 C20 C6 111.01(14) . . ?
N4 C20 H20A 109.4 . . ?
C6 C20 H20A 109.4 . . ?
N4 C20 H20B 109.4 . . ?
C6 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
N4 C21 C22 110.10(14) . . ?
N4 C21 H21A 109.6 . . ?
C22 C21 H21A 109.6 . . ?
N4 C21 H21B 109.6 . . ?
C22 C21 H21B 109.6 . . ?
H21A C21 H21B 108.2 . . ?
C32 C31 C30 118.95(17) . . ?
C32 C31 H31 120.5 . . ?
C30 C31 H31 120.5 . . ?
N6 C32 C31 122.64(17) . . ?
N6 C32 H32 118.7 . . ?
C31 C32 H32 118.7 . . ?
N5 C22 C23 122.22(18) . . ?
N5 C22 C21 115.71(15) . . ?
C23 C22 C21 121.98(17) . . ?
C24 C25 C26 118.83(19) . . ?
C24 C25 H25 120.6 . . ?
C26 C25 H25 120.6 . . ?
C24 C23 C22 118.61(19) . . ?
C24 C23 H23 120.7 . . ?
C22 C23 H23 120.7 . . ?
O2 C33 O3 126.86(16) . . ?
O2 C33 C34 117.48(15) . . ?
O3 C33 C34 115.66(15) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O5 C35 O4 126.85(16) . . ?
O5 C35 C36 116.33(15) . . ?
O4 C35 C36 116.81(15) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C15 N3 C19 118.58(16) . . ?
C15 N3 Ni1 113.31(12) . . ?
C19 N3 Ni1 125.15(12) . . ?
O10 C37 C39 122.2(2) . . ?
O10 C37 C38 121.6(2) . . ?
C39 C37 C38 116.1(2) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 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
O1 Ni2 O3 C33 2.91(15) . . . . ?
O5 Ni2 O3 C33 -87.50(15) . . . . ?
N5 Ni2 O3 C33 -173.11(15) . . . . ?
N6 Ni2 O3 C33 89.40(15) . . . . ?
N4 Ni2 O3 C33 129.8(3) . . . . ?
O1 Ni1 O4 C35 -5.39(15) . . . . ?
O2 Ni1 O4 C35 -96.63(15) . . . . ?
N2 Ni1 O4 C35 177.76(15) . . . . ?
N3 Ni1 O4 C35 81.85(15) . . . . ?
O4 Ni1 O2 C33 53.81(14) . . . . ?
O1 Ni1 O2 C33 -43.18(14) . . . . ?
N2 Ni1 O2 C33 148.89(15) . . . . ?
N1 Ni1 O2 C33 -132.96(14) . . . . ?
O3 Ni2 O1 C1 140.01(12) . . . . ?
O5 Ni2 O1 C1 -123.89(13) . . . . ?
N5 Ni2 O1 C1 -61.0(3) . . . . ?
N6 Ni2 O1 C1 49.13(13) . . . . ?
N4 Ni2 O1 C1 -31.60(13) . . . . ?
O3 Ni2 O1 Ni1 -42.53(7) . . . . ?
O5 Ni2 O1 Ni1 53.56(7) . . . . ?
N5 Ni2 O1 Ni1 116.4(3) . . . . ?
N6 Ni2 O1 Ni1 -133.42(7) . . . . ?
N4 Ni2 O1 Ni1 145.85(7) . . . . ?
O4 Ni1 O1 C1 137.43(12) . . . . ?
O2 Ni1 O1 C1 -128.28(13) . . . . ?
N2 Ni1 O1 C1 -57.0(3) . . . . ?
N3 Ni1 O1 C1 45.70(13) . . . . ?
N1 Ni1 O1 C1 -35.22(13) . . . . ?
O4 Ni1 O1 Ni2 -40.03(7) . . . . ?
O2 Ni1 O1 Ni2 54.26(7) . . . . ?
N2 Ni1 O1 Ni2 125.6(2) . . . . ?
N3 Ni1 O1 Ni2 -131.75(7) . . . . ?
N1 Ni1 O1 Ni2 147.33(7) . . . . ?
O3 Ni2 O5 C35 52.88(15) . . . . ?
O1 Ni2 O5 C35 -42.64(15) . . . . ?
N5 Ni2 O5 C35 147.26(16) . . . . ?
N4 Ni2 O5 C35 -133.46(15) . . . . ?
O3 Ni2 N6 C28 -179.72(11) . . . . ?
O1 Ni2 N6 C28 -84.28(12) . . . . ?
N5 Ni2 N6 C28 85.22(12) . . . . ?
N4 Ni2 N6 C28 7.15(11) . . . . ?
O3 Ni2 N6 C32 -23.81(14) . . . . ?
O1 Ni2 N6 C32 71.63(14) . . . . ?
N5 Ni2 N6 C32 -118.87(14) . . . . ?
N4 Ni2 N6 C32 163.06(14) . . . . ?
O4 Ni1 N2 C13 -11.17(15) . . . . ?
O1 Ni1 N2 C13 -176.82(19) . . . . ?
O2 Ni1 N2 C13 -104.92(15) . . . . ?
N3 Ni1 N2 C13 81.46(15) . . . . ?
N1 Ni1 N2 C13 160.97(15) . . . . ?
O4 Ni1 N2 C9 165.73(12) . . . . ?
O1 Ni1 N2 C9 0.1(3) . . . . ?
O2 Ni1 N2 C9 71.98(12) . . . . ?
N3 Ni1 N2 C9 -101.64(12) . . . . ?
N1 Ni1 N2 C9 -22.13(11) . . . . ?
O3 Ni2 N5 C26 -4.63(15) . . . . ?
O1 Ni2 N5 C26 -163.6(2) . . . . ?
O5 Ni2 N5 C26 -100.35(15) . . . . ?
N6 Ni2 N5 C26 87.24(15) . . . . ?
N4 Ni2 N5 C26 166.41(15) . . . . ?
O3 Ni2 N5 C22 170.64(12) . . . . ?
O1 Ni2 N5 C22 11.6(3) . . . . ?
O5 Ni2 N5 C22 74.92(12) . . . . ?
N6 Ni2 N5 C22 -97.49(12) . . . . ?
N4 Ni2 N5 C22 -18.31(12) . . . . ?
O1 Ni1 N1 C8 -139.08(10) . . . . ?
O2 Ni1 N1 C8 -48.37(10) . . . . ?
N2 Ni1 N1 C8 36.15(10) . . . . ?
N3 Ni1 N1 C8 133.90(10) . . . . ?
O1 Ni1 N1 C14 102.92(10) . . . . ?
O2 Ni1 N1 C14 -166.37(10) . . . . ?
N2 Ni1 N1 C14 -81.85(11) . . . . ?
N3 Ni1 N1 C14 15.90(10) . . . . ?
O1 Ni1 N1 C7 -19.48(11) . . . . ?
O2 Ni1 N1 C7 71.23(11) . . . . ?
N2 Ni1 N1 C7 155.75(12) . . . . ?
N3 Ni1 N1 C7 -106.50(11) . . . . ?
O3 Ni2 N4 C21 91.1(3) . . . . ?
O1 Ni2 N4 C21 -141.71(10) . . . . ?
O5 Ni2 N4 C21 -51.85(10) . . . . ?
N5 Ni2 N4 C21 32.78(10) . . . . ?
N6 Ni2 N4 C21 132.09(11) . . . . ?
O3 Ni2 N4 C27 -27.6(4) . . . . ?
O1 Ni2 N4 C27 99.59(11) . . . . ?
O5 Ni2 N4 C27 -170.56(11) . . . . ?
N5 Ni2 N4 C27 -85.93(11) . . . . ?
N6 Ni2 N4 C27 13.38(11) . . . . ?
O3 Ni2 N4 C20 -149.9(3) . . . . ?
O1 Ni2 N4 C20 -22.70(11) . . . . ?
O5 Ni2 N4 C20 67.15(11) . . . . ?
N5 Ni2 N4 C20 151.78(12) . . . . ?
N6 Ni2 N4 C20 -108.91(11) . . . . ?
C8 N1 C14 C15 -145.34(14) . . . . ?
C7 N1 C14 C15 91.34(16) . . . . ?
Ni1 N1 C14 C15 -31.43(16) . . . . ?
Ni2 O1 C1 C2 -132.46(13) . . . . ?
Ni1 O1 C1 C2 50.23(19) . . . . ?
Ni2 O1 C1 C6 47.8(2) . . . . ?
Ni1 O1 C1 C6 -129.48(14) . . . . ?
C5 C6 C1 O1 -179.29(15) . . . . ?
C20 C6 C1 O1 -0.7(2) . . . . ?
C5 C6 C1 C2 1.0(2) . . . . ?
C20 C6 C1 C2 179.56(15) . . . . ?
C9 N2 C13 C12 0.3(3) . . . . ?
Ni1 N2 C13 C12 177.05(13) . . . . ?
C14 N1 C8 C9 71.33(17) . . . . ?
C7 N1 C8 C9 -165.20(13) . . . . ?
Ni1 N1 C8 C9 -45.02(14) . . . . ?
C2 C3 C4 C5 0.3(3) . . . . ?
C2 C3 C4 Cl1 -179.09(13) . . . . ?
C9 C10 C11 C12 -0.5(3) . . . . ?
C13 N2 C9 C10 -0.3(3) . . . . ?
Ni1 N2 C9 C10 -177.53(13) . . . . ?
C13 N2 C9 C8 179.41(15) . . . . ?
Ni1 N2 C9 C8 2.19(18) . . . . ?
C11 C10 C9 N2 0.4(3) . . . . ?
C11 C10 C9 C8 -179.26(16) . . . . ?
N1 C8 C9 N2 30.0(2) . . . . ?
N1 C8 C9 C10 -150.27(16) . . . . ?
C8 N1 C7 C2 179.36(14) . . . . ?
C14 N1 C7 C2 -57.32(17) . . . . ?
Ni1 N1 C7 C2 63.56(15) . . . . ?
N3 C19 C18 C17 1.6(3) . . . . ?
C1 C6 C5 C4 0.3(3) . . . . ?
C20 C6 C5 C4 -178.20(16) . . . . ?
C3 C4 C5 C6 -1.0(3) . . . . ?
Cl1 C4 C5 C6 178.42(13) . . . . ?
C17 C16 C15 N3 1.9(3) . . . . ?
C17 C16 C15 C14 -174.65(16) . . . . ?
N1 C14 C15 N3 37.1(2) . . . . ?
N1 C14 C15 C16 -146.09(16) . . . . ?
C10 C11 C12 C13 0.5(3) . . . . ?
N2 C13 C12 C11 -0.4(3) . . . . ?
C19 C18 C17 C16 -0.6(3) . . . . ?
C15 C16 C17 C18 -1.1(3) . . . . ?
C4 C3 C2 C1 1.0(2) . . . . ?
C4 C3 C2 C7 -179.95(15) . . . . ?
O1 C1 C2 C3 178.62(15) . . . . ?
C6 C1 C2 C3 -1.7(2) . . . . ?
O1 C1 C2 C7 -0.4(2) . . . . ?
C6 C1 C2 C7 179.26(14) . . . . ?
N1 C7 C2 C3 119.24(17) . . . . ?
N1 C7 C2 C1 -61.70(19) . . . . ?
C32 N6 C28 C29 -1.8(2) . . . . ?
Ni2 N6 C28 C29 155.59(13) . . . . ?
C32 N6 C28 C27 175.76(14) . . . . ?
Ni2 N6 C28 C27 -26.86(17) . . . . ?
C30 C29 C28 N6 1.6(3) . . . . ?
C30 C29 C28 C27 -175.74(16) . . . . ?
C21 N4 C27 C28 -145.23(15) . . . . ?
C20 N4 C27 C28 91.53(17) . . . . ?
Ni2 N4 C27 C28 -30.25(16) . . . . ?
N6 C28 C27 N4 39.0(2) . . . . ?
C29 C28 C27 N4 -143.50(16) . . . . ?
C22 N5 C26 C25 -0.3(3) . . . . ?
Ni2 N5 C26 C25 174.76(14) . . . . ?
C28 C29 C30 C31 -0.1(3) . . . . ?
C21 N4 C20 C6 -178.99(14) . . . . ?
C27 N4 C20 C6 -55.55(18) . . . . ?
Ni2 N4 C20 C6 65.41(15) . . . . ?
C5 C6 C20 N4 116.74(17) . . . . ?
C1 C6 C20 N4 -61.8(2) . . . . ?
C27 N4 C21 C22 75.08(18) . . . . ?
C20 N4 C21 C22 -161.27(14) . . . . ?
Ni2 N4 C21 C22 -42.35(15) . . . . ?
C29 C30 C31 C32 -1.2(3) . . . . ?
C28 N6 C32 C31 0.5(2) . . . . ?
Ni2 N6 C32 C31 -154.20(13) . . . . ?
C30 C31 C32 N6 1.0(3) . . . . ?
C26 N5 C22 C23 -1.9(3) . . . . ?
Ni2 N5 C22 C23 -177.67(14) . . . . ?
C26 N5 C22 C21 174.58(15) . . . . ?
Ni2 N5 C22 C21 -1.17(19) . . . . ?
N4 C21 C22 N5 30.5(2) . . . . ?
N4 C21 C22 C23 -152.98(16) . . . . ?
C23 C24 C25 C26 -0.7(3) . . . . ?
N5 C26 C25 C24 1.6(3) . . . . ?
C25 C24 C23 C22 -1.4(3) . . . . ?
N5 C22 C23 C24 2.8(3) . . . . ?
C21 C22 C23 C24 -173.53(17) . . . . ?
Ni1 O2 C33 O3 10.7(3) . . . . ?
Ni1 O2 C33 C34 -169.16(11) . . . . ?
Ni2 O3 C33 O2 15.3(3) . . . . ?
Ni2 O3 C33 C34 -164.79(11) . . . . ?
Ni2 O5 C35 O4 4.2(3) . . . . ?
Ni2 O5 C35 C36 -176.41(12) . . . . ?
Ni1 O4 C35 O5 26.6(3) . . . . ?
Ni1 O4 C35 C36 -152.79(13) . . . . ?
C16 C15 N3 C19 -1.0(2) . . . . ?
C14 C15 N3 C19 175.78(15) . . . . ?
C16 C15 N3 Ni1 160.54(13) . . . . ?
C14 C15 N3 Ni1 -22.66(18) . . . . ?
C18 C19 N3 C15 -0.8(3) . . . . ?
C18 C19 N3 Ni1 -159.96(14) . . . . ?
O4 Ni1 N3 C15 176.35(12) . . . . ?
O1 Ni1 N3 C15 -86.83(12) . . . . ?
N2 Ni1 N3 C15 80.72(12) . . . . ?
N1 Ni1 N3 C15 3.39(11) . . . . ?
O4 Ni1 N3 C19 -23.51(14) . . . . ?
O1 Ni1 N3 C19 73.31(14) . . . . ?
N2 Ni1 N3 C19 -119.14(14) . . . . ?
N1 Ni1 N3 C19 163.53(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.644
_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/access/V1 
# 
# Audit and citation data items may have 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_RF2623
_database_code_depnum_ccdc_archive 'CCDC 1444960'
_audit_update_record             
;
2015-12-31 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Cu2(LClO-bdpa)(mu2-Oac)(ClO4)]ClO4'
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H33 Cl2 Cu2 N6 O7, Cl O4'
_chemical_formula_sum            'C34 H33 Cl3 Cu2 N6 O11'
_chemical_formula_weight         935.11

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'

_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                   10.6949(4)
_cell_length_b                   20.3869(9)
_cell_length_c                   17.5905(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.489(2)
_cell_angle_gamma                90.00
_cell_volume                     3696.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9798
_cell_measurement_theta_min      2.02
_cell_measurement_theta_max      28.47

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904
_exptl_absorpt_coefficient_mu    1.437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6642
_exptl_absorpt_correction_T_max  0.7922
_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       'φ and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            81476
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         29.06
_reflns_number_total             9835
_reflns_number_gt                7461
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0740P)²+3.5872P] 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         9835
_refine_ls_number_parameters     506
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1363
_refine_ls_wR_factor_gt          0.1099
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.002
_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
Cu1 Cu 0.43000(3) 0.080860(16) 0.38843(2) 0.01458(10) Uani 1 1 d . . .
Cu2 Cu 0.23366(3) 0.222596(17) 0.38811(2) 0.01500(10) Uani 1 1 d . . .
Cl1 Cl 0.88466(7) 0.32140(4) 0.58126(5) 0.02351(16) Uani 1 1 d . . .
Cl3 Cl 0.66660(7) 0.54562(4) 0.36362(5) 0.02768(18) Uani 1 1 d . . .
Cl2 Cl 0.12224(7) 0.13866(4) 0.57529(4) 0.02192(16) Uani 1 1 d . . .
O1 O 0.40661(18) 0.18558(9) 0.41381(12) 0.0155(4) Uani 1 1 d . . .
O3 O 0.26045(19) 0.05540(10) 0.39877(12) 0.0192(4) Uani 1 1 d . . .
O2 O 0.1553(2) 0.14191(10) 0.33410(12) 0.0207(4) Uani 1 1 d . . .
O5 O 0.1665(2) 0.15235(11) 0.50692(13) 0.0264(5) Uani 1 1 d . . .
O9 O 0.6685(3) 0.49279(12) 0.31033(15) 0.0350(6) Uani 1 1 d . . .
O11 O 0.7625(4) 0.53257(15) 0.43518(16) 0.0558(9) Uani 1 1 d . . .
O4 O -0.0124(2) 0.12563(17) 0.55423(17) 0.0494(8) Uani 1 1 d . . .
O7 O 0.1957(3) 0.08791(17) 0.6207(2) 0.0653(11) Uani 1 1 d . . .
O10 O 0.6994(3) 0.60627(13) 0.33176(16) 0.0409(6) Uani 1 1 d . . .
O6 O 0.1419(3) 0.19824(15) 0.62278(16) 0.0485(8) Uani 1 1 d . . .
O8 O 0.5415(3) 0.55176(18) 0.3758(3) 0.0718(11) Uani 1 1 d . . .
C4 C 0.7412(3) 0.28270(13) 0.53006(18) 0.0174(6) Uani 1 1 d . . .
C1 C 0.5133(3) 0.21876(13) 0.45052(17) 0.0146(5) Uani 1 1 d . . .
C6 C 0.5125(3) 0.26472(13) 0.51061(17) 0.0153(5) Uani 1 1 d . . .
C3 C 0.7441(3) 0.23864(14) 0.47076(18) 0.0174(6) Uani 1 1 d . . .
H3 H 0.8232 0.2298 0.4579 0.021 Uiso 1 1 calc R . .
C2 C 0.6297(3) 0.20727(13) 0.42998(17) 0.0163(5) Uani 1 1 d . . .
C5 C 0.6269(3) 0.29662(14) 0.54956(17) 0.0170(5) Uani 1 1 d . . .
H5 H 0.6264 0.3279 0.5895 0.020 Uiso 1 1 calc R . .
C7 C 0.6332(3) 0.16183(13) 0.36331(17) 0.0170(6) Uani 1 1 d . . .
H7A H 0.5641 0.1749 0.3160 0.020 Uiso 1 1 calc R . .
H7B H 0.7175 0.1671 0.3507 0.020 Uiso 1 1 calc R . .
C19 C 0.4536(3) 0.08580(14) 0.56008(18) 0.0182(6) Uani 1 1 d . . .
H19 H 0.3615 0.0835 0.5459 0.022 Uiso 1 1 calc R . .
C12 C 0.2673(3) 0.02884(15) 0.14457(19) 0.0217(6) Uani 1 1 d . . .
H12 H 0.1842 0.0235 0.1086 0.026 Uiso 1 1 calc R . .
C14 C 0.7074(3) 0.07093(14) 0.45617(17) 0.0178(6) Uani 1 1 d . . .
H14A H 0.7880 0.0971 0.4651 0.021 Uiso 1 1 calc R . .
H14B H 0.7302 0.0241 0.4537 0.021 Uiso 1 1 calc R . .
C18 C 0.5190(3) 0.09785(15) 0.63785(19) 0.0223(6) Uani 1 1 d . . .
H18 H 0.4730 0.1041 0.6766 0.027 Uiso 1 1 calc R . .
C13 C 0.2793(3) 0.05080(14) 0.21984(18) 0.0198(6) Uani 1 1 d . . .
H13 H 0.2027 0.0610 0.2350 0.024 Uiso 1 1 calc R . .
C16 C 0.7179(3) 0.09305(15) 0.60008(18) 0.0212(6) Uani 1 1 d . . .
H16 H 0.8099 0.0956 0.6129 0.025 Uiso 1 1 calc R . .
C15 C 0.6464(3) 0.08174(13) 0.52344(18) 0.0168(6) Uani 1 1 d . . .
C10 C 0.4992(3) 0.02273(15) 0.17580(18) 0.0213(6) Uani 1 1 d . . .
H10 H 0.5768 0.0135 0.1613 0.026 Uiso 1 1 calc R . .
C9 C 0.5037(3) 0.04457(13) 0.25095(18) 0.0175(6) Uani 1 1 d . . .
C11 C 0.3792(3) 0.01458(15) 0.12210(18) 0.0220(6) Uani 1 1 d . . .
H11 H 0.3735 -0.0007 0.0703 0.026 Uiso 1 1 calc R . .
C17 C 0.6534(3) 0.10053(16) 0.65782(19) 0.0238(6) Uani 1 1 d . . .
H17 H 0.7009 0.1075 0.7111 0.029 Uiso 1 1 calc R . .
C8 C 0.6306(3) 0.05040(14) 0.31308(18) 0.0186(6) Uani 1 1 d . . .
H8A H 0.6621 0.0061 0.3322 0.022 Uiso 1 1 calc R . .
H8B H 0.6959 0.0709 0.2900 0.022 Uiso 1 1 calc R . .
C22 C 0.0512(3) 0.31175(15) 0.41927(19) 0.0218(6) Uani 1 1 d . . .
C20 C 0.3903(3) 0.27837(14) 0.53465(17) 0.0163(5) Uani 1 1 d . . .
H20A H 0.3631 0.2381 0.5574 0.020 Uiso 1 1 calc R . .
H20B H 0.4074 0.3129 0.5758 0.020 Uiso 1 1 calc R . .
C26 C -0.0414(3) 0.25285(19) 0.3048(2) 0.0304(7) Uani 1 1 d . . .
H26 H -0.0377 0.2173 0.2705 0.036 Uiso 1 1 calc R . .
C23 C -0.0530(3) 0.35486(17) 0.4041(2) 0.0306(8) Uani 1 1 d . . .
H23 H -0.0554 0.3901 0.4391 0.037 Uiso 1 1 calc R . .
C21 C 0.1642(3) 0.31498(15) 0.49106(18) 0.0201(6) Uani 1 1 d . . .
H21A H 0.1703 0.3592 0.5149 0.024 Uiso 1 1 calc R . .
H21B H 0.1534 0.2826 0.5307 0.024 Uiso 1 1 calc R . .
C24 C -0.1543(3) 0.3450(2) 0.3361(3) 0.0404(10) Uani 1 1 d . . .
H24 H -0.2265 0.3740 0.3239 0.049 Uiso 1 1 calc R . .
C25 C -0.1491(3) 0.2937(2) 0.2874(2) 0.0387(9) Uani 1 1 d . . .
H25 H -0.2187 0.2859 0.2419 0.046 Uiso 1 1 calc R . .
C29 C 0.4582(3) 0.38016(15) 0.33192(18) 0.0212(6) Uani 1 1 d . . .
H29 H 0.4957 0.4175 0.3618 0.025 Uiso 1 1 calc R . .
C27 C 0.3210(3) 0.35913(14) 0.42625(18) 0.0185(6) Uani 1 1 d . . .
H27A H 0.3906 0.3832 0.4644 0.022 Uiso 1 1 calc R . .
H27B H 0.2450 0.3887 0.4099 0.022 Uiso 1 1 calc R . .
C32 C 0.3468(3) 0.27261(15) 0.24882(18) 0.0226(6) Uani 1 1 d . . .
H32 H 0.3088 0.2348 0.2203 0.027 Uiso 1 1 calc R . .
C31 C 0.4373(3) 0.30764(16) 0.22231(19) 0.0243(7) Uani 1 1 d . . .
H31 H 0.4609 0.2943 0.1763 0.029 Uiso 1 1 calc R . .
C28 C 0.3671(3) 0.34179(14) 0.35504(17) 0.0179(6) Uani 1 1 d . . .
C30 C 0.4929(3) 0.36242(16) 0.26392(19) 0.0239(6) Uani 1 1 d . . .
H30 H 0.5542 0.3878 0.2463 0.029 Uiso 1 1 calc R . .
C33 C 0.1582(3) 0.08716(15) 0.36778(17) 0.0181(6) Uani 1 1 d . . .
C34 C 0.0310(3) 0.05499(17) 0.3675(2) 0.0275(7) Uani 1 1 d . . .
H34A H -0.0287 0.0880 0.3782 0.041 Uiso 1 1 calc R . .
H34B H 0.0461 0.0210 0.4083 0.041 Uiso 1 1 calc R . .
H34C H -0.0069 0.0351 0.3157 0.041 Uiso 1 1 calc R . .
N1 N 0.6153(2) 0.09082(11) 0.38058(14) 0.0150(5) Uani 1 1 d . . .
N4 N 0.2841(2) 0.30018(11) 0.46594(14) 0.0157(5) Uani 1 1 d . . .
N3 N 0.5163(2) 0.07721(11) 0.50382(15) 0.0162(5) Uani 1 1 d . . .
N2 N 0.3954(2) 0.05867(12) 0.27348(15) 0.0175(5) Uani 1 1 d . . .
N5 N 0.0580(2) 0.26262(13) 0.36928(15) 0.0208(5) Uani 1 1 d . . .
N6 N 0.3103(2) 0.28992(12) 0.31344(15) 0.0191(5) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O3 1.941(2) . ?
Cu1 N3 1.994(3) . ?
Cu1 N2 2.008(2) . ?
Cu1 N1 2.033(2) . ?
Cu1 O1 2.2089(19) . ?
Cu2 O1 1.9362(19) . ?
Cu2 O2 1.971(2) . ?
Cu2 N5 1.993(2) . ?
Cu2 N4 2.067(2) . ?
Cu2 N6 2.204(2) . ?
Cl1 C4 1.746(3) . ?
Cl3 O8 1.415(3) . ?
Cl3 O11 1.420(3) . ?
Cl3 O9 1.432(2) . ?
Cl3 O10 1.439(3) . ?
Cl2 O7 1.411(3) . ?
Cl2 O4 1.413(3) . ?
Cl2 O5 1.432(2) . ?
Cl2 O6 1.457(3) . ?
O1 C1 1.335(3) . ?
O3 C33 1.262(4) . ?
O2 C33 1.260(4) . ?
C4 C3 1.383(4) . ?
C4 C5 1.385(4) . ?
C1 C2 1.406(4) . ?
C1 C6 1.414(4) . ?
C6 C5 1.393(4) . ?
C6 C20 1.503(4) . ?
C3 C2 1.397(4) . ?
C3 H3 0.9500 . ?
C2 C7 1.503(4) . ?
C5 H5 0.9500 . ?
C7 N1 1.502(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C19 N3 1.347(4) . ?
C19 C18 1.382(4) . ?
C19 H19 0.9500 . ?
C12 C13 1.371(4) . ?
C12 C11 1.387(4) . ?
C12 H12 0.9500 . ?
C14 N1 1.484(4) . ?
C14 C15 1.512(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C18 C17 1.387(4) . ?
C18 H18 0.9500 . ?
C13 N2 1.354(4) . ?
C13 H13 0.9500 . ?
C16 C17 1.380(4) . ?
C16 C15 1.380(4) . ?
C16 H16 0.9500 . ?
C15 N3 1.344(4) . ?
C10 C9 1.383(4) . ?
C10 C11 1.385(4) . ?
C10 H10 0.9500 . ?
C9 N2 1.352(4) . ?
C9 C8 1.503(4) . ?
C11 H11 0.9500 . ?
C17 H17 0.9500 . ?
C8 N1 1.490(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C22 N5 1.347(4) . ?
C22 C23 1.388(4) . ?
C22 C21 1.498(4) . ?
C20 N4 1.489(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C26 N5 1.346(4) . ?
C26 C25 1.387(5) . ?
C26 H26 0.9500 . ?
C23 C24 1.397(5) . ?
C23 H23 0.9500 . ?
C21 N4 1.494(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C24 C25 1.363(6) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C29 C28 1.392(4) . ?
C29 C30 1.391(4) . ?
C29 H29 0.9500 . ?
C27 N4 1.495(4) . ?
C27 C28 1.506(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C32 N6 1.344(4) . ?
C32 C31 1.380(4) . ?
C32 H32 0.9500 . ?
C31 C30 1.380(5) . ?
C31 H31 0.9500 . ?
C28 N6 1.336(4) . ?
C30 H30 0.9500 . ?
C33 C34 1.509(4) . ?
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
O3 Cu1 N3 94.85(9) . . ?
O3 Cu1 N2 96.23(9) . . ?
N3 Cu1 N2 158.05(10) . . ?
O3 Cu1 N1 170.10(9) . . ?
N3 Cu1 N1 83.02(10) . . ?
N2 Cu1 N1 82.82(10) . . ?
O3 Cu1 O1 94.61(8) . . ?
N3 Cu1 O1 82.93(8) . . ?
N2 Cu1 O1 114.89(9) . . ?
N1 Cu1 O1 94.72(8) . . ?
O1 Cu2 O2 92.51(8) . . ?
O1 Cu2 N5 176.11(10) . . ?
O2 Cu2 N5 90.06(10) . . ?
O1 Cu2 N4 94.57(9) . . ?
O2 Cu2 N4 163.74(9) . . ?
N5 Cu2 N4 82.21(10) . . ?
O1 Cu2 N6 84.13(9) . . ?
O2 Cu2 N6 114.23(9) . . ?
N5 Cu2 N6 97.47(10) . . ?
N4 Cu2 N6 81.11(9) . . ?
O8 Cl3 O11 111.8(2) . . ?
O8 Cl3 O9 110.17(18) . . ?
O11 Cl3 O9 107.82(18) . . ?
O8 Cl3 O10 108.8(2) . . ?
O11 Cl3 O10 108.21(18) . . ?
O9 Cl3 O10 110.10(16) . . ?
O7 Cl2 O4 112.6(2) . . ?
O7 Cl2 O5 111.07(16) . . ?
O4 Cl2 O5 111.00(16) . . ?
O7 Cl2 O6 108.3(2) . . ?
O4 Cl2 O6 106.75(19) . . ?
O5 Cl2 O6 106.82(16) . . ?
C1 O1 Cu2 123.71(17) . . ?
C1 O1 Cu1 117.34(16) . . ?
Cu2 O1 Cu1 118.83(9) . . ?
C33 O3 Cu1 123.07(19) . . ?
C33 O2 Cu2 123.96(19) . . ?
C3 C4 C5 121.2(3) . . ?
C3 C4 Cl1 119.3(2) . . ?
C5 C4 Cl1 119.5(2) . . ?
O1 C1 C2 119.5(2) . . ?
O1 C1 C6 121.5(2) . . ?
C2 C1 C6 119.0(3) . . ?
C5 C6 C1 119.8(3) . . ?
C5 C6 C20 119.4(3) . . ?
C1 C6 C20 120.8(3) . . ?
C4 C3 C2 119.5(3) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 C7 118.8(2) . . ?
C1 C2 C7 120.8(2) . . ?
C4 C5 C6 120.0(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
N1 C7 C2 113.9(2) . . ?
N1 C7 H7A 108.8 . . ?
C2 C7 H7A 108.8 . . ?
N1 C7 H7B 108.8 . . ?
C2 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
N3 C19 C18 122.1(3) . . ?
N3 C19 H19 119.0 . . ?
C18 C19 H19 119.0 . . ?
C13 C12 C11 118.6(3) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
N1 C14 C15 109.8(2) . . ?
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 . . ?
C17 C18 C19 118.3(3) . . ?
C17 C18 H18 120.8 . . ?
C19 C18 H18 120.8 . . ?
N2 C13 C12 122.9(3) . . ?
N2 C13 H13 118.5 . . ?
C12 C13 H13 118.5 . . ?
C17 C16 C15 118.8(3) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
N3 C15 C16 121.9(3) . . ?
N3 C15 C14 115.0(3) . . ?
C16 C15 C14 123.1(3) . . ?
C9 C10 C11 118.7(3) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
N2 C9 C10 122.3(3) . . ?
N2 C9 C8 116.6(3) . . ?
C10 C9 C8 121.0(3) . . ?
C12 C11 C10 119.5(3) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C16 C17 C18 119.8(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
N1 C8 C9 110.7(2) . . ?
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 . . ?
N5 C22 C23 121.7(3) . . ?
N5 C22 C21 114.3(3) . . ?
C23 C22 C21 124.0(3) . . ?
N4 C20 C6 111.1(2) . . ?
N4 C20 H20A 109.4 . . ?
C6 C20 H20A 109.4 . . ?
N4 C20 H20B 109.4 . . ?
C6 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
N5 C26 C25 121.3(4) . . ?
N5 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C22 C23 C24 118.2(3) . . ?
C22 C23 H23 120.9 . . ?
C24 C23 H23 120.9 . . ?
N4 C21 C22 107.7(2) . . ?
N4 C21 H21A 110.2 . . ?
C22 C21 H21A 110.2 . . ?
N4 C21 H21B 110.2 . . ?
C22 C21 H21B 110.2 . . ?
H21A C21 H21B 108.5 . . ?
C25 C24 C23 119.7(3) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 119.5(4) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C28 C29 C30 118.2(3) . . ?
C28 C29 H29 120.9 . . ?
C30 C29 H29 120.9 . . ?
N4 C27 C28 112.7(2) . . ?
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 . . ?
N6 C32 C31 122.6(3) . . ?
N6 C32 H32 118.7 . . ?
C31 C32 H32 118.7 . . ?
C32 C31 C30 118.8(3) . . ?
C32 C31 H31 120.6 . . ?
C30 C31 H31 120.6 . . ?
N6 C28 C29 122.4(3) . . ?
N6 C28 C27 116.0(2) . . ?
C29 C28 C27 121.4(3) . . ?
C31 C30 C29 119.4(3) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
O2 C33 O3 124.5(3) . . ?
O2 C33 C34 118.3(3) . . ?
O3 C33 C34 117.0(3) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C14 N1 C8 112.0(2) . . ?
C14 N1 C7 110.8(2) . . ?
C8 N1 C7 109.0(2) . . ?
C14 N1 Cu1 109.74(17) . . ?
C8 N1 Cu1 108.39(17) . . ?
C7 N1 Cu1 106.81(16) . . ?
C20 N4 C21 110.4(2) . . ?
C20 N4 C27 112.3(2) . . ?
C21 N4 C27 109.3(2) . . ?
C20 N4 Cu2 108.46(17) . . ?
C21 N4 Cu2 104.93(17) . . ?
C27 N4 Cu2 111.14(18) . . ?
C19 N3 C15 119.1(3) . . ?
C19 N3 Cu1 123.9(2) . . ?
C15 N3 Cu1 115.12(19) . . ?
C9 N2 C13 118.0(3) . . ?
C9 N2 Cu1 113.66(19) . . ?
C13 N2 Cu1 128.1(2) . . ?
C26 N5 C22 119.5(3) . . ?
C26 N5 Cu2 125.2(2) . . ?
C22 N5 Cu2 114.1(2) . . ?
C28 N6 C32 118.6(3) . . ?
C28 N6 Cu2 110.71(19) . . ?
C32 N6 Cu2 125.4(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C6 C5 177.6(3) . . . . ?
C2 C1 C6 C5 -1.5(4) . . . . ?
O1 C1 C6 C20 -0.7(4) . . . . ?
C2 C1 C6 C20 -179.8(3) . . . . ?
C5 C4 C3 C2 -0.3(4) . . . . ?
Cl1 C4 C3 C2 179.6(2) . . . . ?
C4 C3 C2 C1 -1.9(4) . . . . ?
C4 C3 C2 C7 177.3(3) . . . . ?
O1 C1 C2 C3 -176.3(3) . . . . ?
C6 C1 C2 C3 2.8(4) . . . . ?
O1 C1 C2 C7 4.5(4) . . . . ?
C6 C1 C2 C7 -176.4(3) . . . . ?
C3 C4 C5 C6 1.7(4) . . . . ?
Cl1 C4 C5 C6 -178.2(2) . . . . ?
C1 C6 C5 C4 -0.8(4) . . . . ?
C20 C6 C5 C4 177.6(3) . . . . ?
C3 C2 C7 N1 110.7(3) . . . . ?
C1 C2 C7 N1 -70.0(3) . . . . ?
N3 C19 C18 C17 -0.5(4) . . . . ?
C11 C12 C13 N2 -0.6(5) . . . . ?
C17 C16 C15 N3 -0.7(4) . . . . ?
C17 C16 C15 C14 -178.2(3) . . . . ?
N1 C14 C15 N3 28.6(3) . . . . ?
N1 C14 C15 C16 -153.7(3) . . . . ?
C11 C10 C9 N2 -0.5(5) . . . . ?
C11 C10 C9 C8 176.3(3) . . . . ?
C13 C12 C11 C10 0.1(5) . . . . ?
C9 C10 C11 C12 0.5(5) . . . . ?
C15 C16 C17 C18 -1.2(5) . . . . ?
C19 C18 C17 C16 1.8(5) . . . . ?
N2 C9 C8 N1 -18.1(4) . . . . ?
C10 C9 C8 N1 164.9(3) . . . . ?
C5 C6 C20 N4 124.7(3) . . . . ?
C1 C6 C20 N4 -56.9(3) . . . . ?
N5 C22 C23 C24 1.9(5) . . . . ?
C21 C22 C23 C24 -177.9(3) . . . . ?
N5 C22 C21 N4 39.7(3) . . . . ?
C23 C22 C21 N4 -140.5(3) . . . . ?
C22 C23 C24 C25 0.7(5) . . . . ?
C23 C24 C25 C26 -1.8(6) . . . . ?
N5 C26 C25 C24 0.5(6) . . . . ?
N6 C32 C31 C30 0.2(5) . . . . ?
C30 C29 C28 N6 -1.6(4) . . . . ?
C30 C29 C28 C27 -177.8(3) . . . . ?
N4 C27 C28 N6 33.9(4) . . . . ?
N4 C27 C28 C29 -149.7(3) . . . . ?
C32 C31 C30 C29 1.2(5) . . . . ?
C28 C29 C30 C31 -0.5(4) . . . . ?
C15 C14 N1 C8 -148.0(2) . . . . ?
C15 C14 N1 C7 90.2(3) . . . . ?
C15 C14 N1 Cu1 -27.5(3) . . . . ?
C9 C8 N1 C14 150.1(2) . . . . ?
C9 C8 N1 C7 -87.0(3) . . . . ?
C9 C8 N1 Cu1 28.9(3) . . . . ?
C2 C7 N1 C14 -52.1(3) . . . . ?
C2 C7 N1 C8 -175.7(2) . . . . ?
C2 C7 N1 Cu1 67.4(3) . . . . ?
C22 C21 N4 C20 -159.1(2) . . . . ?
C22 C21 N4 C27 76.8(3) . . . . ?
C22 C21 N4 Cu2 -42.4(2) . . . . ?
C28 C27 N4 C20 97.4(3) . . . . ?
C28 C27 N4 C21 -139.7(2) . . . . ?
C28 C27 N4 Cu2 -24.3(3) . . . . ?
C18 C19 N3 C15 -1.3(4) . . . . ?
C18 C19 N3 Cu1 -164.9(2) . . . . ?
C16 C15 N3 C19 1.9(4) . . . . ?
C14 C15 N3 C19 179.7(2) . . . . ?
C16 C15 N3 Cu1 166.9(2) . . . . ?
C14 C15 N3 Cu1 -15.4(3) . . . . ?
C10 C9 N2 C13 0.1(4) . . . . ?
C8 C9 N2 C13 -176.9(3) . . . . ?
C10 C9 N2 Cu1 174.4(2) . . . . ?
C8 C9 N2 Cu1 -2.5(3) . . . . ?
C12 C13 N2 C9 0.5(4) . . . . ?
C12 C13 N2 Cu1 -172.9(2) . . . . ?
C25 C26 N5 C22 2.0(5) . . . . ?
C25 C26 N5 Cu2 -164.6(3) . . . . ?
C23 C22 N5 C26 -3.2(5) . . . . ?
C21 C22 N5 C26 176.6(3) . . . . ?
C23 C22 N5 Cu2 164.8(2) . . . . ?
C21 C22 N5 Cu2 -15.4(3) . . . . ?
C29 C28 N6 C32 3.0(4) . . . . ?
C27 C28 N6 C32 179.3(3) . . . . ?
C29 C28 N6 Cu2 158.6(2) . . . . ?
C27 C28 N6 Cu2 -25.0(3) . . . . ?
C31 C32 N6 C28 -2.3(5) . . . . ?
C31 C32 N6 Cu2 -154.1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.327
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.175
####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_R2621
_database_code_depnum_ccdc_archive 'CCDC 1444961'
_audit_update_record             
;
2015-12-31 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            Cu2(L-Cl-O-bdpa)(acetato)2]PF6.H2O
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H36 Cl Cu2 N6 O5, F6 P, H2 O'
_chemical_formula_sum            'C36 H38 Cl Cu2 F6 N6 O6 P'
_chemical_formula_weight         958.24

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'
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   '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                   11.0390(2)
_cell_length_b                   27.5883(6)
_cell_length_c                   12.7990(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.3270(10)
_cell_angle_gamma                90.00
_cell_volume                     3897.84(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9900
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      28.92

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1952
_exptl_absorpt_coefficient_mu    1.284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7481
_exptl_absorpt_correction_T_max  0.8612
_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       'φ and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44754
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         29.04
_reflns_number_total             10374
_reflns_number_gt                7776
_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)+(0.0473P)²+1.5163P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10374
_refine_ls_number_parameters     533
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0988
_refine_ls_wR_factor_gt          0.0785
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu2 Cu 0.68035(2) 0.146372(9) 0.72471(2) 0.01227(7) Uani 1 1 d . . .
Cu1 Cu 0.33164(2) 0.152742(9) 0.78676(2) 0.01278(7) Uani 1 1 d . . .
P1 P 0.02796(6) 0.10427(2) 0.26798(5) 0.02019(13) Uani 1 1 d . . .
O1 O 0.50392(13) 0.11492(5) 0.76032(11) 0.0139(3) Uani 1 1 d . . .
F1 F -0.11651(13) 0.09821(6) 0.26523(12) 0.0363(4) Uani 1 1 d . . .
F6 F 0.03605(14) 0.07641(6) 0.15805(12) 0.0338(4) Uani 1 1 d . . .
F3 F 0.17239(12) 0.10942(5) 0.27014(12) 0.0286(3) Uani 1 1 d . . .
F4 F 0.04074(15) 0.05314(5) 0.32739(13) 0.0369(4) Uani 1 1 d . . .
F2 F 0.01754(15) 0.15433(6) 0.20716(14) 0.0391(4) Uani 1 1 d . . .
F5 F 0.01976(14) 0.13130(6) 0.37742(12) 0.0358(4) Uani 1 1 d . . .
Cl1 Cl 0.49052(6) -0.09755(2) 0.79415(5) 0.02900(15) Uani 1 1 d . . .
C1 C 0.50144(18) 0.06732(8) 0.76768(17) 0.0144(4) Uani 1 1 d . . .
C2 C 0.44248(19) 0.04415(8) 0.85265(17) 0.0152(4) Uani 1 1 d . . .
C3 C 0.4403(2) -0.00623(8) 0.85961(18) 0.0181(5) Uani 1 1 d . . .
H3 H 0.4014 -0.0214 0.9170 0.022 Uiso 1 1 calc R . .
C6 C 0.5566(2) 0.03744(8) 0.69176(17) 0.0159(4) Uani 1 1 d . . .
C4 C 0.4944(2) -0.03427(8) 0.78358(19) 0.0204(5) Uani 1 1 d . . .
C5 C 0.5527(2) -0.01276(8) 0.70040(18) 0.0193(5) Uani 1 1 d . . .
H5 H 0.5904 -0.0324 0.6489 0.023 Uiso 1 1 calc R . .
C7 C 0.3853(2) 0.07456(8) 0.93543(17) 0.0165(4) Uani 1 1 d . . .
H7A H 0.4464 0.0975 0.9633 0.020 Uiso 1 1 calc R . .
H7B H 0.3595 0.0533 0.9936 0.020 Uiso 1 1 calc R . .
C9 C 0.2034(2) 0.06745(8) 0.73058(19) 0.0182(5) Uani 1 1 d . . .
C12 C 0.2213(2) 0.07201(9) 0.5185(2) 0.0262(5) Uani 1 1 d . . .
H12 H 0.2275 0.0745 0.4447 0.031 Uiso 1 1 calc R . .
C11 C 0.1671(2) 0.03202(10) 0.5642(2) 0.0297(6) Uani 1 1 d . . .
H11 H 0.1354 0.0067 0.5219 0.036 Uiso 1 1 calc R . .
C13 C 0.2660(2) 0.10808(9) 0.58235(18) 0.0201(5) Uani 1 1 d . . .
H13 H 0.3053 0.1352 0.5517 0.024 Uiso 1 1 calc R . .
C10 C 0.1594(2) 0.02925(9) 0.6719(2) 0.0259(5) Uani 1 1 d . . .
H10 H 0.1247 0.0017 0.7046 0.031 Uiso 1 1 calc R . .
C8 C 0.1862(2) 0.07025(9) 0.84766(19) 0.0209(5) Uani 1 1 d . . .
H8A H 0.1040 0.0826 0.8629 0.025 Uiso 1 1 calc R . .
H8B H 0.1934 0.0374 0.8781 0.025 Uiso 1 1 calc R . .
C18 C 0.4424(2) 0.25763(9) 1.0136(2) 0.0254(5) Uani 1 1 d . . .
H18 H 0.4881 0.2868 1.0160 0.030 Uiso 1 1 calc R . .
C19 C 0.4209(2) 0.23467(8) 0.91969(19) 0.0198(5) Uani 1 1 d . . .
H19 H 0.4534 0.2482 0.8576 0.024 Uiso 1 1 calc R . .
C15 C 0.3071(2) 0.17511(8) 1.00151(18) 0.0189(5) Uani 1 1 d . . .
C14 C 0.2280(2) 0.13130(9) 0.98445(19) 0.0219(5) Uani 1 1 d . . .
H14A H 0.2262 0.1113 1.0486 0.026 Uiso 1 1 calc R . .
H14B H 0.1441 0.1416 0.9680 0.026 Uiso 1 1 calc R . .
C17 C 0.3966(2) 0.23773(10) 1.1045(2) 0.0281(6) Uani 1 1 d . . .
H17 H 0.4124 0.2526 1.1701 0.034 Uiso 1 1 calc R . .
C16 C 0.3274(2) 0.19583(9) 1.09865(19) 0.0248(5) Uani 1 1 d . . .
H16 H 0.2946 0.1817 1.1599 0.030 Uiso 1 1 calc R . .
C20 C 0.6178(2) 0.06085(8) 0.60020(17) 0.0165(4) Uani 1 1 d . . .
H20A H 0.6404 0.0354 0.5493 0.020 Uiso 1 1 calc R . .
H20B H 0.5598 0.0830 0.5653 0.020 Uiso 1 1 calc R . .
C23 C 0.8622(2) 0.03293(9) 0.87359(19) 0.0220(5) Uani 1 1 d . . .
H23 H 0.8992 0.0039 0.8499 0.026 Uiso 1 1 calc R . .
C22 C 0.80894(19) 0.06486(8) 0.80346(18) 0.0155(4) Uani 1 1 d . . .
C25 C 0.8015(2) 0.08571(9) 1.01260(18) 0.0217(5) Uani 1 1 d . . .
H25 H 0.7981 0.0936 1.0848 0.026 Uiso 1 1 calc R . .
C21 C 0.8183(2) 0.05796(8) 0.68692(18) 0.0184(5) Uani 1 1 d . . .
H21A H 0.9012 0.0664 0.6640 0.022 Uiso 1 1 calc R . .
H21B H 0.8036 0.0235 0.6695 0.022 Uiso 1 1 calc R . .
C24 C 0.8603(2) 0.04425(9) 0.9788(2) 0.0247(5) Uani 1 1 d . . .
H24 H 0.8993 0.0236 1.0279 0.030 Uiso 1 1 calc R . .
C26 C 0.7482(2) 0.11517(8) 0.93868(17) 0.0173(5) Uani 1 1 d . . .
H26 H 0.7059 0.1433 0.9611 0.021 Uiso 1 1 calc R . .
C27 C 0.7817(2) 0.11145(9) 0.53544(18) 0.0206(5) Uani 1 1 d . . .
H27A H 0.7833 0.0877 0.4775 0.025 Uiso 1 1 calc R . .
H27B H 0.8659 0.1220 0.5499 0.025 Uiso 1 1 calc R . .
C28 C 0.7049(2) 0.15434(9) 0.50557(18) 0.0197(5) Uani 1 1 d . . .
C29 C 0.6850(2) 0.16899(10) 0.40354(19) 0.0269(6) Uani 1 1 d . . .
H29 H 0.7177 0.1512 0.3468 0.032 Uiso 1 1 calc R . .
C30 C 0.6164(2) 0.21025(11) 0.3860(2) 0.0311(6) Uani 1 1 d . . .
H30 H 0.6009 0.2209 0.3167 0.037 Uiso 1 1 calc R . .
C32 C 0.5930(2) 0.21918(9) 0.57002(19) 0.0208(5) Uani 1 1 d . . .
H32 H 0.5618 0.2367 0.6278 0.025 Uiso 1 1 calc R . .
C31 C 0.5706(2) 0.23581(10) 0.4697(2) 0.0259(6) Uani 1 1 d . . .
H31 H 0.5244 0.2644 0.4586 0.031 Uiso 1 1 calc R . .
N1 N 0.27777(17) 0.10267(7) 0.89646(15) 0.0162(4) Uani 1 1 d . . .
N3 N 0.35550(17) 0.19366(7) 0.91338(14) 0.0168(4) Uani 1 1 d . . .
N2 N 0.25556(16) 0.10609(7) 0.68688(14) 0.0156(4) Uani 1 1 d . . .
N5 N 0.75394(16) 0.10554(6) 0.83580(14) 0.0139(4) Uani 1 1 d . . .
N4 N 0.72898(16) 0.08881(7) 0.63035(14) 0.0151(4) Uani 1 1 d . . .
N6 N 0.65784(16) 0.17887(7) 0.58726(15) 0.0167(4) Uani 1 1 d . . .
C35 C 0.7527(2) 0.22847(8) 0.83716(16) 0.0152(4) Uani 1 1 d . . .
C33 C 0.2605(2) 0.23083(8) 0.67133(16) 0.0150(4) Uani 1 1 d . . .
C36 C 0.7305(2) 0.27890(8) 0.87917(19) 0.0222(5) Uani 1 1 d . . .
H36A H 0.6949 0.2767 0.9490 0.033 Uiso 1 1 calc R . .
H36B H 0.6748 0.2962 0.8324 0.033 Uiso 1 1 calc R . .
H36C H 0.8075 0.2965 0.8834 0.033 Uiso 1 1 calc R . .
C34 C 0.2803(2) 0.28063(9) 0.62502(19) 0.0226(5) Uani 1 1 d . . .
H34A H 0.2020 0.2947 0.6052 0.034 Uiso 1 1 calc R . .
H34B H 0.3316 0.2779 0.5631 0.034 Uiso 1 1 calc R . .
H34C H 0.3201 0.3015 0.6768 0.034 Uiso 1 1 calc R . .
O5 O 0.85718(14) 0.21185(6) 0.83811(13) 0.0208(4) Uani 1 1 d . . .
O2 O 0.35688(14) 0.20659(6) 0.69206(12) 0.0178(3) Uani 1 1 d . . .
O3 O 0.15659(15) 0.21656(6) 0.68833(14) 0.0236(4) Uani 1 1 d . . .
O4 O 0.65954(14) 0.20588(6) 0.80313(12) 0.0182(3) Uani 1 1 d . . .
O6 O 0.9938(2) 0.14331(7) 0.7366(2) 0.0385(6) Uani 1 1 d . . .
H1O H 1.041(3) 0.1579(12) 0.716(3) 0.042(11) Uiso 1 1 d . . .
H2O H 0.956(3) 0.1600(12) 0.774(3) 0.043(10) Uiso 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu2 O4 1.9385(16) . ?
Cu2 N5 1.9843(18) . ?
Cu2 N6 1.9888(18) . ?
Cu2 N4 2.0678(18) . ?
Cu2 O1 2.1826(14) . ?
Cu1 O2 1.9384(15) . ?
Cu1 N3 1.9913(19) . ?
Cu1 N2 1.9959(18) . ?
Cu1 N1 2.0599(18) . ?
Cu1 O1 2.1972(14) . ?
P1 F2 1.5893(16) . ?
P1 F5 1.5900(16) . ?
P1 F3 1.6009(15) . ?
P1 F1 1.6037(16) . ?
P1 F6 1.6061(16) . ?
P1 F4 1.6082(16) . ?
O1 C1 1.317(3) . ?
Cl1 C4 1.752(2) . ?
C1 C6 1.415(3) . ?
C1 C2 1.422(3) . ?
C2 C3 1.393(3) . ?
C2 C7 1.494(3) . ?
C3 C4 1.382(3) . ?
C3 H3 0.9500 . ?
C6 C5 1.390(3) . ?
C6 C20 1.502(3) . ?
C4 C5 1.381(3) . ?
C5 H5 0.9500 . ?
C7 N1 1.501(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 N2 1.336(3) . ?
C9 C10 1.381(3) . ?
C9 C8 1.513(3) . ?
C12 C13 1.377(3) . ?
C12 C11 1.386(4) . ?
C12 H12 0.9500 . ?
C11 C10 1.383(4) . ?
C11 H11 0.9500 . ?
C13 N2 1.345(3) . ?
C13 H13 0.9500 . ?
C10 H10 0.9500 . ?
C8 N1 1.485(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C18 C19 1.378(3) . ?
C18 C17 1.384(4) . ?
C18 H18 0.9500 . ?
C19 N3 1.344(3) . ?
C19 H19 0.9500 . ?
C15 N3 1.351(3) . ?
C15 C16 1.386(3) . ?
C15 C14 1.507(3) . ?
C14 N1 1.484(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C17 C16 1.387(4) . ?
C17 H17 0.9500 . ?
C16 H16 0.9500 . ?
C20 N4 1.498(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C23 C24 1.383(4) . ?
C23 C22 1.386(3) . ?
C23 H23 0.9500 . ?
C22 N5 1.343(3) . ?
C22 C21 1.508(3) . ?
C25 C26 1.377(3) . ?
C25 C24 1.386(4) . ?
C25 H25 0.9500 . ?
C21 N4 1.487(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C24 H24 0.9500 . ?
C26 N5 1.345(3) . ?
C26 H26 0.9500 . ?
C27 N4 1.488(3) . ?
C27 C28 1.504(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 N6 1.352(3) . ?
C28 C29 1.383(3) . ?
C29 C30 1.385(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.381(4) . ?
C30 H30 0.9500 . ?
C32 N6 1.340(3) . ?
C32 C31 1.384(3) . ?
C32 H32 0.9500 . ?
C31 H31 0.9500 . ?
C35 O5 1.241(3) . ?
C35 O4 1.277(3) . ?
C35 C36 1.512(3) . ?
C33 O3 1.234(3) . ?
C33 O2 1.283(3) . ?
C33 C34 1.513(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O6 H1O 0.71(3) . ?
O6 H2O 0.79(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Cu2 N5 99.15(7) . . ?
O4 Cu2 N6 93.54(7) . . ?
N5 Cu2 N6 159.77(8) . . ?
O4 Cu2 N4 169.96(7) . . ?
N5 Cu2 N4 82.87(7) . . ?
N6 Cu2 N4 82.02(8) . . ?
O4 Cu2 O1 96.90(6) . . ?
N5 Cu2 O1 89.25(6) . . ?
N6 Cu2 O1 104.88(6) . . ?
N4 Cu2 O1 92.96(6) . . ?
O2 Cu1 N3 93.19(7) . . ?
O2 Cu1 N2 98.93(7) . . ?
N3 Cu1 N2 160.06(8) . . ?
O2 Cu1 N1 169.51(7) . . ?
N3 Cu1 N1 82.12(8) . . ?
N2 Cu1 N1 83.23(8) . . ?
O2 Cu1 O1 98.05(6) . . ?
N3 Cu1 O1 106.50(7) . . ?
N2 Cu1 O1 87.51(6) . . ?
N1 Cu1 O1 92.29(6) . . ?
F2 P1 F5 91.12(9) . . ?
F2 P1 F3 90.03(9) . . ?
F5 P1 F3 90.27(8) . . ?
F2 P1 F1 90.61(9) . . ?
F5 P1 F1 90.38(9) . . ?
F3 P1 F1 179.08(10) . . ?
F2 P1 F6 89.49(9) . . ?
F5 P1 F6 179.38(10) . . ?
F3 P1 F6 89.85(8) . . ?
F1 P1 F6 89.49(9) . . ?
F2 P1 F4 178.61(11) . . ?
F5 P1 F4 90.01(9) . . ?
F3 P1 F4 89.14(9) . . ?
F1 P1 F4 90.20(9) . . ?
F6 P1 F4 89.39(9) . . ?
C1 O1 Cu2 115.49(13) . . ?
C1 O1 Cu1 116.37(13) . . ?
Cu2 O1 Cu1 128.13(7) . . ?
O1 C1 C6 121.5(2) . . ?
O1 C1 C2 120.8(2) . . ?
C6 C1 C2 117.7(2) . . ?
C3 C2 C1 120.4(2) . . ?
C3 C2 C7 120.5(2) . . ?
C1 C2 C7 119.1(2) . . ?
C4 C3 C2 120.4(2) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C5 C6 C1 120.8(2) . . ?
C5 C6 C20 120.3(2) . . ?
C1 C6 C20 118.9(2) . . ?
C5 C4 C3 120.5(2) . . ?
C5 C4 Cl1 119.97(19) . . ?
C3 C4 Cl1 119.52(19) . . ?
C4 C5 C6 120.3(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C2 C7 N1 113.02(18) . . ?
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 . . ?
N2 C9 C10 122.1(2) . . ?
N2 C9 C8 115.5(2) . . ?
C10 C9 C8 122.2(2) . . ?
C13 C12 C11 118.6(2) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C10 C11 C12 119.6(2) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
N2 C13 C12 121.9(2) . . ?
N2 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
C9 C10 C11 118.5(2) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 H10 120.8 . . ?
N1 C8 C9 111.00(18) . . ?
N1 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C19 C18 C17 119.3(2) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
N3 C19 C18 121.9(2) . . ?
N3 C19 H19 119.0 . . ?
C18 C19 H19 119.0 . . ?
N3 C15 C16 122.0(2) . . ?
N3 C15 C14 114.5(2) . . ?
C16 C15 C14 123.5(2) . . ?
N1 C14 C15 108.65(18) . . ?
N1 C14 H14A 110.0 . . ?
C15 C14 H14A 110.0 . . ?
N1 C14 H14B 110.0 . . ?
C15 C14 H14B 110.0 . . ?
H14A C14 H14B 108.3 . . ?
C18 C17 C16 119.3(2) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C15 C16 C17 118.6(2) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
N4 C20 C6 113.07(17) . . ?
N4 C20 H20A 109.0 . . ?
C6 C20 H20A 109.0 . . ?
N4 C20 H20B 109.0 . . ?
C6 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C24 C23 C22 118.6(2) . . ?
C24 C23 H23 120.7 . . ?
C22 C23 H23 120.7 . . ?
N5 C22 C23 121.5(2) . . ?
N5 C22 C21 116.36(19) . . ?
C23 C22 C21 122.0(2) . . ?
C26 C25 C24 118.2(2) . . ?
C26 C25 H25 120.9 . . ?
C24 C25 H25 120.9 . . ?
N4 C21 C22 111.12(18) . . ?
N4 C21 H21A 109.4 . . ?
C22 C21 H21A 109.4 . . ?
N4 C21 H21B 109.4 . . ?
C22 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C23 C24 C25 120.0(2) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
N5 C26 C25 122.3(2) . . ?
N5 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
N4 C27 C28 108.38(18) . . ?
N4 C27 H27A 110.0 . . ?
C28 C27 H27A 110.0 . . ?
N4 C27 H27B 110.0 . . ?
C28 C27 H27B 110.0 . . ?
H27A C27 H27B 108.4 . . ?
N6 C28 C29 121.6(2) . . ?
N6 C28 C27 114.6(2) . . ?
C29 C28 C27 123.8(2) . . ?
C28 C29 C30 118.5(2) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
C31 C30 C29 119.8(2) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
N6 C32 C31 121.3(2) . . ?
N6 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C30 C31 C32 119.1(2) . . ?
C30 C31 H31 120.5 . . ?
C32 C31 H31 120.5 . . ?
C14 N1 C8 112.68(18) . . ?
C14 N1 C7 108.58(18) . . ?
C8 N1 C7 111.34(17) . . ?
C14 N1 Cu1 105.67(14) . . ?
C8 N1 Cu1 108.40(14) . . ?
C7 N1 Cu1 110.01(13) . . ?
C19 N3 C15 118.9(2) . . ?
C19 N3 Cu1 126.47(16) . . ?
C15 N3 Cu1 114.42(15) . . ?
C9 N2 C13 119.2(2) . . ?
C9 N2 Cu1 115.29(15) . . ?
C13 N2 Cu1 124.96(16) . . ?
C22 N5 C26 119.39(19) . . ?
C22 N5 Cu2 115.96(15) . . ?
C26 N5 Cu2 124.61(15) . . ?
C21 N4 C27 112.10(17) . . ?
C21 N4 C20 111.74(17) . . ?
C27 N4 C20 109.25(17) . . ?
C21 N4 Cu2 109.19(13) . . ?
C27 N4 Cu2 104.99(14) . . ?
C20 N4 Cu2 109.32(13) . . ?
C32 N6 C28 119.7(2) . . ?
C32 N6 Cu2 125.70(16) . . ?
C28 N6 Cu2 114.32(16) . . ?
O5 C35 O4 124.7(2) . . ?
O5 C35 C36 119.3(2) . . ?
O4 C35 C36 116.0(2) . . ?
O3 C33 O2 124.6(2) . . ?
O3 C33 C34 119.7(2) . . ?
O2 C33 C34 115.67(19) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 O2 Cu1 114.01(14) . . ?
C35 O4 Cu2 119.49(14) . . ?
H1O O6 H2O 107(4) . . ?

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
O4 Cu2 O1 C1 -147.20(14) . . . . ?
N5 Cu2 O1 C1 -48.07(14) . . . . ?
N6 Cu2 O1 C1 117.27(14) . . . . ?
N4 Cu2 O1 C1 34.75(14) . . . . ?
O4 Cu2 O1 Cu1 32.13(9) . . . . ?
N5 Cu2 O1 Cu1 131.25(9) . . . . ?
N6 Cu2 O1 Cu1 -63.41(10) . . . . ?
N4 Cu2 O1 Cu1 -145.93(9) . . . . ?
O2 Cu1 O1 C1 -147.71(14) . . . . ?
N3 Cu1 O1 C1 116.53(14) . . . . ?
N2 Cu1 O1 C1 -49.04(14) . . . . ?
N1 Cu1 O1 C1 34.07(15) . . . . ?
O2 Cu1 O1 Cu2 32.97(10) . . . . ?
N3 Cu1 O1 Cu2 -62.79(10) . . . . ?
N2 Cu1 O1 Cu2 131.64(10) . . . . ?
N1 Cu1 O1 Cu2 -145.24(9) . . . . ?
Cu2 O1 C1 C6 -47.0(2) . . . . ?
Cu1 O1 C1 C6 133.60(17) . . . . ?
Cu2 O1 C1 C2 133.19(17) . . . . ?
Cu1 O1 C1 C2 -46.2(2) . . . . ?
O1 C1 C2 C3 179.95(19) . . . . ?
C6 C1 C2 C3 0.1(3) . . . . ?
O1 C1 C2 C7 -1.4(3) . . . . ?
C6 C1 C2 C7 178.82(19) . . . . ?
C1 C2 C3 C4 -0.6(3) . . . . ?
C7 C2 C3 C4 -179.3(2) . . . . ?
O1 C1 C6 C5 -179.71(19) . . . . ?
C2 C1 C6 C5 0.1(3) . . . . ?
O1 C1 C6 C20 -0.8(3) . . . . ?
C2 C1 C6 C20 179.01(19) . . . . ?
C2 C3 C4 C5 0.9(3) . . . . ?
C2 C3 C4 Cl1 179.98(17) . . . . ?
C3 C4 C5 C6 -0.6(4) . . . . ?
Cl1 C4 C5 C6 -179.74(17) . . . . ?
C1 C6 C5 C4 0.1(3) . . . . ?
C20 C6 C5 C4 -178.8(2) . . . . ?
C3 C2 C7 N1 -114.2(2) . . . . ?
C1 C2 C7 N1 67.1(3) . . . . ?
C13 C12 C11 C10 -0.1(4) . . . . ?
C11 C12 C13 N2 -1.8(4) . . . . ?
N2 C9 C10 C11 -1.8(3) . . . . ?
C8 C9 C10 C11 172.9(2) . . . . ?
C12 C11 C10 C9 1.8(4) . . . . ?
N2 C9 C8 N1 -26.7(3) . . . . ?
C10 C9 C8 N1 158.3(2) . . . . ?
C17 C18 C19 N3 0.8(4) . . . . ?
N3 C15 C14 N1 34.1(3) . . . . ?
C16 C15 C14 N1 -147.4(2) . . . . ?
C19 C18 C17 C16 -1.7(4) . . . . ?
N3 C15 C16 C17 2.0(3) . . . . ?
C14 C15 C16 C17 -176.5(2) . . . . ?
C18 C17 C16 C15 0.4(4) . . . . ?
C5 C6 C20 N4 -113.8(2) . . . . ?
C1 C6 C20 N4 67.3(3) . . . . ?
C24 C23 C22 N5 -1.4(3) . . . . ?
C24 C23 C22 C21 173.5(2) . . . . ?
N5 C22 C21 N4 -19.5(3) . . . . ?
C23 C22 C21 N4 165.3(2) . . . . ?
C22 C23 C24 C25 2.7(3) . . . . ?
C26 C25 C24 C23 -1.3(3) . . . . ?
C24 C25 C26 N5 -1.6(3) . . . . ?
N4 C27 C28 N6 35.0(3) . . . . ?
N4 C27 C28 C29 -146.5(2) . . . . ?
N6 C28 C29 C30 0.9(4) . . . . ?
C27 C28 C29 C30 -177.5(2) . . . . ?
C28 C29 C30 C31 0.5(4) . . . . ?
C29 C30 C31 C32 -0.9(4) . . . . ?
N6 C32 C31 C30 -0.1(4) . . . . ?
C15 C14 N1 C8 -158.57(18) . . . . ?
C15 C14 N1 C7 77.6(2) . . . . ?
C15 C14 N1 Cu1 -40.4(2) . . . . ?
C9 C8 N1 C14 143.2(2) . . . . ?
C9 C8 N1 C7 -94.5(2) . . . . ?
C9 C8 N1 Cu1 26.6(2) . . . . ?
C2 C7 N1 C14 179.80(18) . . . . ?
C2 C7 N1 C8 55.2(2) . . . . ?
C2 C7 N1 Cu1 -65.0(2) . . . . ?
O2 Cu1 N1 C14 -35.0(5) . . . . ?
N3 Cu1 N1 C14 28.95(14) . . . . ?
N2 Cu1 N1 C14 -137.49(15) . . . . ?
O1 Cu1 N1 C14 135.29(14) . . . . ?
O2 Cu1 N1 C8 86.0(4) . . . . ?
N3 Cu1 N1 C8 149.97(15) . . . . ?
N2 Cu1 N1 C8 -16.47(14) . . . . ?
O1 Cu1 N1 C8 -103.69(14) . . . . ?
O2 Cu1 N1 C7 -152.0(3) . . . . ?
N3 Cu1 N1 C7 -88.07(14) . . . . ?
N2 Cu1 N1 C7 105.49(14) . . . . ?
O1 Cu1 N1 C7 18.27(14) . . . . ?
C18 C19 N3 C15 1.5(3) . . . . ?
C18 C19 N3 Cu1 -173.01(17) . . . . ?
C16 C15 N3 C19 -2.9(3) . . . . ?
C14 C15 N3 C19 175.6(2) . . . . ?
C16 C15 N3 Cu1 172.26(17) . . . . ?
C14 C15 N3 Cu1 -9.2(2) . . . . ?
O2 Cu1 N3 C19 -26.35(19) . . . . ?
N2 Cu1 N3 C19 -153.9(2) . . . . ?
N1 Cu1 N3 C19 163.1(2) . . . . ?
O1 Cu1 N3 C19 73.01(19) . . . . ?
O2 Cu1 N3 C15 158.89(16) . . . . ?
N2 Cu1 N3 C15 31.4(3) . . . . ?
N1 Cu1 N3 C15 -11.68(15) . . . . ?
O1 Cu1 N3 C15 -101.74(16) . . . . ?
C10 C9 N2 C13 -0.1(3) . . . . ?
C8 C9 N2 C13 -175.1(2) . . . . ?
C10 C9 N2 Cu1 -172.33(17) . . . . ?
C8 C9 N2 Cu1 12.6(2) . . . . ?
C12 C13 N2 C9 1.9(3) . . . . ?
C12 C13 N2 Cu1 173.35(17) . . . . ?
O2 Cu1 N2 C9 -167.18(15) . . . . ?
N3 Cu1 N2 C9 -40.5(3) . . . . ?
N1 Cu1 N2 C9 2.45(16) . . . . ?
O1 Cu1 N2 C9 95.05(15) . . . . ?
O2 Cu1 N2 C13 21.04(19) . . . . ?
N3 Cu1 N2 C13 147.7(2) . . . . ?
N1 Cu1 N2 C13 -169.33(19) . . . . ?
O1 Cu1 N2 C13 -76.72(18) . . . . ?
C23 C22 N5 C26 -1.3(3) . . . . ?
C21 C22 N5 C26 -176.53(19) . . . . ?
C23 C22 N5 Cu2 -179.02(17) . . . . ?
C21 C22 N5 Cu2 5.8(2) . . . . ?
C25 C26 N5 C22 2.9(3) . . . . ?
C25 C26 N5 Cu2 -179.65(17) . . . . ?
O4 Cu2 N5 C22 -163.96(15) . . . . ?
N6 Cu2 N5 C22 -35.8(3) . . . . ?
N4 Cu2 N5 C22 6.10(15) . . . . ?
O1 Cu2 N5 C22 99.18(15) . . . . ?
O4 Cu2 N5 C26 18.47(18) . . . . ?
N6 Cu2 N5 C26 146.6(2) . . . . ?
N4 Cu2 N5 C26 -171.47(18) . . . . ?
O1 Cu2 N5 C26 -78.40(18) . . . . ?
C22 C21 N4 C27 138.63(19) . . . . ?
C22 C21 N4 C20 -98.3(2) . . . . ?
C22 C21 N4 Cu2 22.7(2) . . . . ?
C28 C27 N4 C21 -160.05(18) . . . . ?
C28 C27 N4 C20 75.5(2) . . . . ?
C28 C27 N4 Cu2 -41.63(19) . . . . ?
C6 C20 N4 C21 56.6(2) . . . . ?
C6 C20 N4 C27 -178.82(18) . . . . ?
C6 C20 N4 Cu2 -64.4(2) . . . . ?
O4 Cu2 N4 C21 86.2(4) . . . . ?
N5 Cu2 N4 C21 -16.11(14) . . . . ?
N6 Cu2 N4 C21 150.40(15) . . . . ?
O1 Cu2 N4 C21 -104.98(14) . . . . ?
O4 Cu2 N4 C27 -34.2(5) . . . . ?
N5 Cu2 N4 C27 -136.48(14) . . . . ?
N6 Cu2 N4 C27 30.03(14) . . . . ?
O1 Cu2 N4 C27 134.65(13) . . . . ?
O4 Cu2 N4 C20 -151.3(4) . . . . ?
N5 Cu2 N4 C20 106.42(14) . . . . ?
N6 Cu2 N4 C20 -87.07(14) . . . . ?
O1 Cu2 N4 C20 17.55(14) . . . . ?
C31 C32 N6 C28 1.5(3) . . . . ?
C31 C32 N6 Cu2 -172.12(17) . . . . ?
C29 C28 N6 C32 -1.9(3) . . . . ?
C27 C28 N6 C32 176.6(2) . . . . ?
C29 C28 N6 Cu2 172.40(18) . . . . ?
C27 C28 N6 Cu2 -9.1(2) . . . . ?
O4 Cu2 N6 C32 -27.59(19) . . . . ?
N5 Cu2 N6 C32 -156.5(2) . . . . ?
N4 Cu2 N6 C32 161.46(19) . . . . ?
O1 Cu2 N6 C32 70.51(19) . . . . ?
O4 Cu2 N6 C28 158.49(16) . . . . ?
N5 Cu2 N6 C28 29.6(3) . . . . ?
N4 Cu2 N6 C28 -12.46(16) . . . . ?
O1 Cu2 N6 C28 -103.41(16) . . . . ?
O3 C33 O2 Cu1 -15.9(3) . . . . ?
C34 C33 O2 Cu1 162.78(15) . . . . ?
N3 Cu1 O2 C33 -87.22(15) . . . . ?
N2 Cu1 O2 C33 76.88(15) . . . . ?
N1 Cu1 O2 C33 -24.2(5) . . . . ?
O1 Cu1 O2 C33 165.61(14) . . . . ?
O5 C35 O4 Cu2 -11.5(3) . . . . ?
C36 C35 O4 Cu2 168.81(15) . . . . ?
N5 Cu2 O4 C35 64.40(16) . . . . ?
N6 Cu2 O4 C35 -99.79(16) . . . . ?
N4 Cu2 O4 C35 -36.5(5) . . . . ?
O1 Cu2 O4 C35 154.75(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        29.04
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.156
####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_s2622a
_database_code_depnum_ccdc_archive 'CCDC 1444962'
_audit_update_record             
;
2015-12-31 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Zn2(L-Cl-O-bdpa)(mu-acetato)2]PF6'
_chemical_formula_moiety         'C36 H36 Cl N6 O5 Zn2, F6 P'
_chemical_formula_sum            'C36 H36 Cl F6 N6 O5 P Zn2'
_chemical_formula_weight         943.91

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'
Cl Cl 0.1484 0.1585 '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'
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'
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'

_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                   10.2050(14)
_cell_length_b                   12.0710(17)
_cell_length_c                   16.930(2)
_cell_angle_alpha                90.53(2)
_cell_angle_beta                 106.84(2)
_cell_angle_gamma                104.35(2)
_cell_volume                     1926.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.30
_cell_measurement_theta_max      26.00

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6486
_exptl_absorpt_correction_T_max  0.8134
_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       'φ and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15176
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.26
_diffrn_reflns_theta_max         26.32
_reflns_number_total             7674
_reflns_number_gt                6975
_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)+(0.0267P)²+4.9541P] 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         7674
_refine_ls_number_parameters     516
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1101
_refine_ls_wR_factor_gt          0.1079
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_restrained_S_all      1.197
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.61228(4) 0.38500(3) 0.29884(3) 0.01545(11) Uani 1 1 d . . .
Zn2 Zn 0.90433(4) 0.28428(4) 0.33193(3) 0.01541(11) Uani 1 1 d . . .
Cl1 Cl 0.57456(11) 0.14997(8) -0.10196(6) 0.0258(2) Uani 1 1 d . . .
O1 O 0.7253(3) 0.3017(2) 0.24938(15) 0.0163(5) Uani 1 1 d . . .
O2 O 0.7918(3) 0.5190(2) 0.35264(16) 0.0203(6) Uani 1 1 d . . .
O3 O 0.9778(3) 0.4427(2) 0.39029(16) 0.0198(6) Uani 1 1 d . . .
O4 O 0.6127(3) 0.3009(2) 0.40109(16) 0.0213(6) Uani 1 1 d . . .
O5 O 0.7706(3) 0.1982(2) 0.40542(16) 0.0196(6) Uani 1 1 d . . .
N1 N 0.5584(3) 0.4663(3) 0.17972(18) 0.0155(6) Uani 1 1 d . . .
N2 N 0.4950(3) 0.5004(3) 0.32223(19) 0.0178(6) Uani 1 1 d . . .
N3 N 0.4204(3) 0.2565(3) 0.2218(2) 0.0203(7) Uani 1 1 d . . .
N4 N 0.8755(3) 0.1174(3) 0.26430(19) 0.0185(7) Uani 1 1 d . . .
N5 N 1.0623(3) 0.2169(3) 0.41139(19) 0.0175(6) Uani 1 1 d . . .
N6 N 1.0128(3) 0.3362(3) 0.23610(19) 0.0174(6) Uani 1 1 d . . .
C1 C 0.9203(4) 0.5255(3) 0.3833(2) 0.0170(7) Uani 1 1 d . . .
C2 C 1.0198(4) 0.6428(3) 0.4149(2) 0.0212(8) Uani 1 1 d . . .
H2A H 0.9670 0.7013 0.4016 0.032 Uiso 1 1 calc R . .
H2B H 1.0955 0.6573 0.3887 0.032 Uiso 1 1 calc R . .
H2C H 1.0612 0.6461 0.4751 0.032 Uiso 1 1 calc R . .
C7 C 0.6720(4) 0.2226(3) 0.4261(2) 0.0178(8) Uani 1 1 d . . .
C8 C 0.6148(4) 0.1492(3) 0.4871(3) 0.0259(9) Uani 1 1 d . . .
H8A H 0.5523 0.0759 0.4582 0.039 Uiso 1 1 calc R . .
H8B H 0.5613 0.1893 0.5114 0.039 Uiso 1 1 calc R . .
H8C H 0.6940 0.1349 0.5311 0.039 Uiso 1 1 calc R . .
C10 C 0.6907(4) 0.2675(3) 0.1699(2) 0.0156(7) Uani 1 1 d . . .
C11 C 1.0401(4) 0.1025(3) 0.3991(2) 0.0196(8) Uani 1 1 d . . .
C13 C 0.6873(4) 0.1540(3) 0.1448(2) 0.0173(8) Uani 1 1 d . . .
C15 C 0.6246(4) 0.3070(3) 0.0262(2) 0.0182(8) Uani 1 1 d . . .
H15 H 0.6042 0.3583 -0.0151 0.022 Uiso 1 1 calc R . .
C17 C 0.7262(4) 0.0746(3) 0.2109(2) 0.0180(8) Uani 1 1 d . . .
H17A H 0.6620 0.0669 0.2457 0.022 Uiso 1 1 calc R . .
H17B H 0.7127 -0.0024 0.1842 0.022 Uiso 1 1 calc R . .
C21 C 0.6506(4) 0.1186(3) 0.0617(2) 0.0185(8) Uani 1 1 d . . .
H21 H 0.6466 0.0423 0.0448 0.022 Uiso 1 1 calc R . .
C22 C 0.6591(4) 0.3435(3) 0.1087(2) 0.0169(7) Uani 1 1 d . . .
C23 C 0.4139(4) 0.4053(3) 0.1277(2) 0.0193(8) Uani 1 1 d . . .
H23A H 0.4077 0.4119 0.0686 0.023 Uiso 1 1 calc R . .
H23B H 0.3443 0.4421 0.1398 0.023 Uiso 1 1 calc R . .
C25 C 0.3765(4) 0.2798(3) 0.1431(2) 0.0197(8) Uani 1 1 d . . .
C27 C 0.3389(4) 0.6538(3) 0.3329(3) 0.0236(8) Uani 1 1 d . . .
H27 H 0.2847 0.7063 0.3363 0.028 Uiso 1 1 calc R . .
C29 C 0.2948(4) 0.1956(3) 0.0794(3) 0.0237(8) Uani 1 1 d . . .
H29 H 0.2668 0.2144 0.0237 0.028 Uiso 1 1 calc R . .
C32 C 0.9100(4) 0.0414(3) 0.3298(2) 0.0211(8) Uani 1 1 d . . .
H32A H 0.9271 -0.0273 0.3064 0.025 Uiso 1 1 calc R . .
H32B H 0.8288 0.0155 0.3520 0.025 Uiso 1 1 calc R . .
C33 C 1.0392(4) 0.4426(3) 0.2126(2) 0.0204(8) Uani 1 1 d . . .
H33 H 1.0481 0.5044 0.2506 0.025 Uiso 1 1 calc R . .
C34 C 0.2991(4) 0.0590(4) 0.1805(3) 0.0277(9) Uani 1 1 d . . .
H34 H 0.2726 -0.0172 0.1955 0.033 Uiso 1 1 calc R . .
C35 C 1.0390(4) 0.3769(4) 0.0800(2) 0.0246(9) Uani 1 1 d . . .
H35 H 1.0477 0.3908 0.0264 0.029 Uiso 1 1 calc R . .
C36 C 0.5655(4) 0.5843(3) 0.2069(2) 0.0187(8) Uani 1 1 d . . .
H36A H 0.5237 0.6234 0.1586 0.022 Uiso 1 1 calc R . .
H36B H 0.6658 0.6275 0.2321 0.022 Uiso 1 1 calc R . .
C41 C 1.0107(4) 0.2662(3) 0.1032(2) 0.0202(8) Uani 1 1 d . . .
H41 H 0.9990 0.2029 0.0658 0.024 Uiso 1 1 calc R . .
C46 C 0.3507(4) 0.5710(4) 0.3881(2) 0.0244(9) Uani 1 1 d . . .
H46 H 0.3062 0.5660 0.4305 0.029 Uiso 1 1 calc R . .
C48 C 0.4856(4) 0.5826(3) 0.2694(2) 0.0168(7) Uani 1 1 d . . .
C50 C 0.4066(4) 0.6600(3) 0.2725(2) 0.0203(8) Uani 1 1 d . . .
H50 H 0.3991 0.7163 0.2338 0.024 Uiso 1 1 calc R . .
C53 C 0.6648(4) 0.4642(3) 0.1359(2) 0.0175(7) Uani 1 1 d . . .
H53A H 0.7609 0.5016 0.1731 0.021 Uiso 1 1 calc R . .
H53B H 0.6469 0.5086 0.0868 0.021 Uiso 1 1 calc R . .
C54 C 1.0543(4) 0.4672(3) 0.1356(2) 0.0218(8) Uani 1 1 d . . .
H54 H 1.0748 0.5441 0.1214 0.026 Uiso 1 1 calc R . .
C55 C 0.6198(4) 0.1952(3) 0.0036(2) 0.0193(8) Uani 1 1 d . . .
C56 C 1.1731(4) 0.2748(3) 0.4741(2) 0.0209(8) Uani 1 1 d . . .
H56 H 1.1885 0.3555 0.4825 0.025 Uiso 1 1 calc R . .
C58 C 1.2424(4) 0.1061(4) 0.5142(3) 0.0276(9) Uani 1 1 d . . .
H58 H 1.3040 0.0679 0.5500 0.033 Uiso 1 1 calc R . .
C59 C 1.1296(4) 0.0442(4) 0.4494(3) 0.0246(9) Uani 1 1 d . . .
H59 H 1.1137 -0.0363 0.4396 0.029 Uiso 1 1 calc R . .
C62 C 0.4292(4) 0.4951(3) 0.3801(2) 0.0205(8) Uani 1 1 d . . .
H62 H 0.4364 0.4369 0.4173 0.025 Uiso 1 1 calc R . .
C63 C 0.9996(4) 0.2491(3) 0.1824(2) 0.0181(8) Uani 1 1 d . . .
C64 C 0.2554(4) 0.0839(4) 0.0991(3) 0.0303(10) Uani 1 1 d . . .
H64 H 0.1986 0.0246 0.0569 0.036 Uiso 1 1 calc R . .
C66 C 0.9752(4) 0.1315(3) 0.2141(2) 0.0193(8) Uani 1 1 d . . .
H66A H 0.9361 0.0722 0.1666 0.023 Uiso 1 1 calc R . .
H66B H 1.0669 0.1203 0.2484 0.023 Uiso 1 1 calc R . .
C68 C 1.2653(4) 0.2232(4) 0.5268(2) 0.0252(9) Uani 1 1 d . . .
H68 H 1.3428 0.2670 0.5707 0.030 Uiso 1 1 calc R . .
C71 C 0.3818(4) 0.1472(3) 0.2393(3) 0.0236(8) Uani 1 1 d . . .
H71 H 0.4133 0.1300 0.2952 0.028 Uiso 1 1 calc R . .
P1 P 0.96814(11) 0.78383(9) 0.16529(7) 0.0219(2) Uani 1 1 d . . .
F1 F 1.0606(3) 0.8768(2) 0.24178(16) 0.0353(6) Uani 1 1 d . . .
F2 F 0.9582(3) 0.6852(2) 0.22667(16) 0.0421(7) Uani 1 1 d . . .
F3 F 1.1106(3) 0.7608(2) 0.1561(2) 0.0492(8) Uani 1 1 d . . .
F4 F 0.9783(3) 0.8822(2) 0.10372(17) 0.0458(7) Uani 1 1 d . . .
F5 F 0.8762(3) 0.6906(2) 0.08870(15) 0.0349(6) Uani 1 1 d . . .
F6 F 0.8267(3) 0.8070(2) 0.1749(2) 0.0485(8) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 2.014(3) . ?
Zn1 O1 2.040(2) . ?
Zn1 O2 2.083(3) . ?
Zn1 N2 2.150(3) . ?
Zn1 N3 2.218(3) . ?
Zn1 N1 2.235(3) . ?
Zn2 O3 2.005(3) . ?
Zn2 O1 2.013(2) . ?
Zn2 N5 2.118(3) . ?
Zn2 O5 2.190(3) . ?
Zn2 N4 2.219(3) . ?
Zn2 N6 2.228(3) . ?
Cl1 C55 1.755(4) . ?
O1 C10 1.323(4) . ?
O2 C1 1.245(4) . ?
O3 C1 1.269(4) . ?
O4 C7 1.258(4) . ?
O5 C7 1.254(4) . ?
N1 C36 1.470(4) . ?
N1 C23 1.480(4) . ?
N1 C53 1.487(4) . ?
N2 C62 1.332(5) . ?
N2 C48 1.345(5) . ?
N3 C25 1.332(5) . ?
N3 C71 1.343(5) . ?
N4 C32 1.466(5) . ?
N4 C66 1.485(5) . ?
N4 C17 1.486(5) . ?
N5 C56 1.339(5) . ?
N5 C11 1.346(5) . ?
N6 C33 1.334(5) . ?
N6 C63 1.339(5) . ?
C1 C2 1.510(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C7 C8 1.517(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 C22 1.409(5) . ?
C10 C13 1.419(5) . ?
C11 C59 1.391(5) . ?
C11 C32 1.509(5) . ?
C13 C21 1.381(5) . ?
C13 C17 1.510(5) . ?
C15 C22 1.378(5) . ?
C15 C55 1.384(5) . ?
C15 H15 0.9500 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C21 C55 1.380(5) . ?
C21 H21 0.9500 . ?
C22 C53 1.507(5) . ?
C23 C25 1.513(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C25 C29 1.389(5) . ?
C27 C46 1.378(6) . ?
C27 C50 1.384(5) . ?
C27 H27 0.9500 . ?
C29 C64 1.382(6) . ?
C29 H29 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C54 1.382(5) . ?
C33 H33 0.9500 . ?
C34 C71 1.373(6) . ?
C34 C64 1.381(6) . ?
C34 H34 0.9500 . ?
C35 C41 1.381(6) . ?
C35 C54 1.381(6) . ?
C35 H35 0.9500 . ?
C36 C48 1.509(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C41 C63 1.390(5) . ?
C41 H41 0.9500 . ?
C46 C62 1.387(5) . ?
C46 H46 0.9500 . ?
C48 C50 1.386(5) . ?
C50 H50 0.9500 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54 0.9500 . ?
C56 C68 1.373(5) . ?
C56 H56 0.9500 . ?
C58 C68 1.379(6) . ?
C58 C59 1.383(6) . ?
C58 H58 0.9500 . ?
C59 H59 0.9500 . ?
C62 H62 0.9500 . ?
C63 C66 1.510(5) . ?
C64 H64 0.9500 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C68 H68 0.9500 . ?
C71 H71 0.9500 . ?
P1 F6 1.588(3) . ?
P1 F4 1.591(3) . ?
P1 F2 1.591(3) . ?
P1 F3 1.596(3) . ?
P1 F1 1.602(3) . ?
P1 F5 1.604(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Zn1 O1 99.85(10) . . ?
O4 Zn1 O2 97.33(11) . . ?
O1 Zn1 O2 91.64(10) . . ?
O4 Zn1 N2 96.02(11) . . ?
O1 Zn1 N2 164.11(11) . . ?
O2 Zn1 N2 85.44(11) . . ?
O4 Zn1 N3 92.41(12) . . ?
O1 Zn1 N3 86.36(11) . . ?
O2 Zn1 N3 170.25(11) . . ?
N2 Zn1 N3 93.89(11) . . ?
O4 Zn1 N1 166.94(11) . . ?
O1 Zn1 N1 87.76(10) . . ?
O2 Zn1 N1 93.01(11) . . ?
N2 Zn1 N1 76.82(11) . . ?
N3 Zn1 N1 77.39(11) . . ?
O3 Zn2 O1 99.60(10) . . ?
O3 Zn2 N5 95.41(11) . . ?
O1 Zn2 N5 163.98(11) . . ?
O3 Zn2 O5 100.95(10) . . ?
O1 Zn2 O5 87.03(10) . . ?
N5 Zn2 O5 84.66(11) . . ?
O3 Zn2 N4 166.08(11) . . ?
O1 Zn2 N4 89.12(11) . . ?
N5 Zn2 N4 77.26(12) . . ?
O5 Zn2 N4 90.25(11) . . ?
O3 Zn2 N6 92.01(11) . . ?
O1 Zn2 N6 87.40(10) . . ?
N5 Zn2 N6 97.66(11) . . ?
O5 Zn2 N6 166.59(10) . . ?
N4 Zn2 N6 77.48(11) . . ?
C10 O1 Zn2 122.0(2) . . ?
C10 O1 Zn1 124.1(2) . . ?
Zn2 O1 Zn1 113.71(11) . . ?
C1 O2 Zn1 134.3(2) . . ?
C1 O3 Zn2 129.9(2) . . ?
C7 O4 Zn1 128.1(2) . . ?
C7 O5 Zn2 132.2(2) . . ?
C36 N1 C23 111.5(3) . . ?
C36 N1 C53 111.5(3) . . ?
C23 N1 C53 110.9(3) . . ?
C36 N1 Zn1 103.1(2) . . ?
C23 N1 Zn1 109.7(2) . . ?
C53 N1 Zn1 109.9(2) . . ?
C62 N2 C48 119.0(3) . . ?
C62 N2 Zn1 126.9(3) . . ?
C48 N2 Zn1 114.1(2) . . ?
C25 N3 C71 117.9(3) . . ?
C25 N3 Zn1 114.0(2) . . ?
C71 N3 Zn1 123.6(3) . . ?
C32 N4 C66 110.8(3) . . ?
C32 N4 C17 111.2(3) . . ?
C66 N4 C17 110.9(3) . . ?
C32 N4 Zn2 104.3(2) . . ?
C66 N4 Zn2 109.5(2) . . ?
C17 N4 Zn2 109.9(2) . . ?
C56 N5 C11 118.6(3) . . ?
C56 N5 Zn2 126.7(3) . . ?
C11 N5 Zn2 114.6(2) . . ?
C33 N6 C63 118.4(3) . . ?
C33 N6 Zn2 123.3(2) . . ?
C63 N6 Zn2 113.6(2) . . ?
O2 C1 O3 126.4(3) . . ?
O2 C1 C2 117.8(3) . . ?
O3 C1 C2 115.8(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O5 C7 O4 127.3(3) . . ?
O5 C7 C8 117.2(3) . . ?
O4 C7 C8 115.5(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 C10 C22 120.7(3) . . ?
O1 C10 C13 120.4(3) . . ?
C22 C10 C13 118.9(3) . . ?
N5 C11 C59 121.6(4) . . ?
N5 C11 C32 116.1(3) . . ?
C59 C11 C32 122.3(3) . . ?
C21 C13 C10 120.1(3) . . ?
C21 C13 C17 121.4(3) . . ?
C10 C13 C17 118.5(3) . . ?
C22 C15 C55 119.7(3) . . ?
C22 C15 H15 120.1 . . ?
C55 C15 H15 120.1 . . ?
N4 C17 C13 111.9(3) . . ?
N4 C17 H17A 109.2 . . ?
C13 C17 H17A 109.2 . . ?
N4 C17 H17B 109.2 . . ?
C13 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C55 C21 C13 119.4(3) . . ?
C55 C21 H21 120.3 . . ?
C13 C21 H21 120.3 . . ?
C15 C22 C10 120.0(3) . . ?
C15 C22 C53 121.4(3) . . ?
C10 C22 C53 118.6(3) . . ?
N1 C23 C25 111.7(3) . . ?
N1 C23 H23A 109.3 . . ?
C25 C23 H23A 109.3 . . ?
N1 C23 H23B 109.3 . . ?
C25 C23 H23B 109.3 . . ?
H23A C23 H23B 107.9 . . ?
N3 C25 C29 122.7(4) . . ?
N3 C25 C23 115.8(3) . . ?
C29 C25 C23 121.5(4) . . ?
C46 C27 C50 119.5(4) . . ?
C46 C27 H27 120.3 . . ?
C50 C27 H27 120.3 . . ?
C64 C29 C25 118.3(4) . . ?
C64 C29 H29 120.9 . . ?
C25 C29 H29 120.9 . . ?
N4 C32 C11 110.8(3) . . ?
N4 C32 H32A 109.5 . . ?
C11 C32 H32A 109.5 . . ?
N4 C32 H32B 109.5 . . ?
C11 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
N6 C33 C54 123.2(4) . . ?
N6 C33 H33 118.4 . . ?
C54 C33 H33 118.4 . . ?
C71 C34 C64 118.2(4) . . ?
C71 C34 H34 120.9 . . ?
C64 C34 H34 120.9 . . ?
C41 C35 C54 119.2(4) . . ?
C41 C35 H35 120.4 . . ?
C54 C35 H35 120.4 . . ?
N1 C36 C48 110.1(3) . . ?
N1 C36 H36A 109.6 . . ?
C48 C36 H36A 109.6 . . ?
N1 C36 H36B 109.6 . . ?
C48 C36 H36B 109.6 . . ?
H36A C36 H36B 108.2 . . ?
C35 C41 C63 118.8(4) . . ?
C35 C41 H41 120.6 . . ?
C63 C41 H41 120.6 . . ?
C27 C46 C62 118.3(4) . . ?
C27 C46 H46 120.8 . . ?
C62 C46 H46 120.8 . . ?
N2 C48 C50 121.7(3) . . ?
N2 C48 C36 115.7(3) . . ?
C50 C48 C36 122.7(3) . . ?
C27 C50 C48 118.9(4) . . ?
C27 C50 H50 120.6 . . ?
C48 C50 H50 120.6 . . ?
N1 C53 C22 111.7(3) . . ?
N1 C53 H53A 109.3 . . ?
C22 C53 H53A 109.3 . . ?
N1 C53 H53B 109.3 . . ?
C22 C53 H53B 109.3 . . ?
H53A C53 H53B 107.9 . . ?
C35 C54 C33 118.3(4) . . ?
C35 C54 H54 120.9 . . ?
C33 C54 H54 120.9 . . ?
C21 C55 C15 121.8(3) . . ?
C21 C55 Cl1 119.1(3) . . ?
C15 C55 Cl1 119.1(3) . . ?
N5 C56 C68 123.2(4) . . ?
N5 C56 H56 118.4 . . ?
C68 C56 H56 118.4 . . ?
C68 C58 C59 120.0(4) . . ?
C68 C58 H58 120.0 . . ?
C59 C58 H58 120.0 . . ?
C58 C59 C11 118.5(4) . . ?
C58 C59 H59 120.7 . . ?
C11 C59 H59 120.7 . . ?
N2 C62 C46 122.6(4) . . ?
N2 C62 H62 118.7 . . ?
C46 C62 H62 118.7 . . ?
N6 C63 C41 122.1(3) . . ?
N6 C63 C66 115.6(3) . . ?
C41 C63 C66 122.3(3) . . ?
C34 C64 C29 119.5(4) . . ?
C34 C64 H64 120.2 . . ?
C29 C64 H64 120.2 . . ?
N4 C66 C63 111.3(3) . . ?
N4 C66 H66A 109.4 . . ?
C63 C66 H66A 109.4 . . ?
N4 C66 H66B 109.4 . . ?
C63 C66 H66B 109.4 . . ?
H66A C66 H66B 108.0 . . ?
C56 C68 C58 118.1(4) . . ?
C56 C68 H68 120.9 . . ?
C58 C68 H68 120.9 . . ?
N3 C71 C34 123.3(4) . . ?
N3 C71 H71 118.3 . . ?
C34 C71 H71 118.3 . . ?
F6 P1 F4 90.24(17) . . ?
F6 P1 F2 89.93(17) . . ?
F4 P1 F2 179.79(17) . . ?
F6 P1 F3 179.69(18) . . ?
F4 P1 F3 89.91(17) . . ?
F2 P1 F3 89.92(17) . . ?
F6 P1 F1 90.20(15) . . ?
F4 P1 F1 89.64(15) . . ?
F2 P1 F1 90.49(14) . . ?
F3 P1 F1 89.53(15) . . ?
F6 P1 F5 90.05(15) . . ?
F4 P1 F5 90.39(14) . . ?
F2 P1 F5 89.48(14) . . ?
F3 P1 F5 90.22(15) . . ?
F1 P1 F5 179.75(15) . . ?

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
C56 N5 C11 C59 -0.3(5) . . . . ?
C56 N5 C11 C32 177.4(3) . . . . ?
O1 C10 C13 C21 179.7(3) . . . . ?
C22 C10 C13 C21 -1.3(5) . . . . ?
O1 C10 C13 C17 -1.0(5) . . . . ?
C22 C10 C13 C17 177.9(3) . . . . ?
C32 N4 C17 C13 178.0(3) . . . . ?
C66 N4 C17 C13 -58.2(4) . . . . ?
C21 C13 C17 N4 116.5(4) . . . . ?
C10 C13 C17 N4 -62.7(4) . . . . ?
C10 C13 C21 C55 1.1(5) . . . . ?
C17 C13 C21 C55 -178.1(3) . . . . ?
C55 C15 C22 C10 0.6(5) . . . . ?
C55 C15 C22 C53 -179.7(3) . . . . ?
O1 C10 C22 C15 179.4(3) . . . . ?
C13 C10 C22 C15 0.5(5) . . . . ?
O1 C10 C22 C53 -0.3(5) . . . . ?
C13 C10 C22 C53 -179.2(3) . . . . ?
C36 N1 C23 C25 -143.9(3) . . . . ?
C53 N1 C23 C25 91.2(4) . . . . ?
C71 N3 C25 C29 -0.9(5) . . . . ?
C71 N3 C25 C23 175.7(3) . . . . ?
N1 C23 C25 N3 39.4(4) . . . . ?
N1 C23 C25 C29 -144.0(3) . . . . ?
N3 C25 C29 C64 1.5(6) . . . . ?
C23 C25 C29 C64 -174.9(3) . . . . ?
C66 N4 C32 C11 75.0(4) . . . . ?
C17 N4 C32 C11 -161.2(3) . . . . ?
N5 C11 C32 N4 29.8(4) . . . . ?
C59 C11 C32 N4 -152.5(3) . . . . ?
C63 N6 C33 C54 -0.3(5) . . . . ?
C23 N1 C36 C48 70.2(4) . . . . ?
C53 N1 C36 C48 -165.2(3) . . . . ?
C54 C35 C41 C63 -0.5(5) . . . . ?
C50 C27 C46 C62 -0.9(6) . . . . ?
C62 N2 C48 C50 -1.5(5) . . . . ?
C62 N2 C48 C36 178.8(3) . . . . ?
N1 C36 C48 N2 36.6(4) . . . . ?
N1 C36 C48 C50 -143.0(3) . . . . ?
C46 C27 C50 C48 -0.4(6) . . . . ?
N2 C48 C50 C27 1.7(6) . . . . ?
C36 C48 C50 C27 -178.7(3) . . . . ?
C36 N1 C53 C22 179.3(3) . . . . ?
C23 N1 C53 C22 -55.7(4) . . . . ?
C15 C22 C53 N1 117.4(4) . . . . ?
C10 C22 C53 N1 -62.9(4) . . . . ?
C41 C35 C54 C33 -0.7(5) . . . . ?
N6 C33 C54 C35 1.1(6) . . . . ?
C13 C21 C55 C15 0.0(5) . . . . ?
C13 C21 C55 Cl1 179.5(3) . . . . ?
C22 C15 C55 C21 -0.9(5) . . . . ?
C22 C15 C55 Cl1 179.6(3) . . . . ?
C11 N5 C56 C68 -0.2(5) . . . . ?
C68 C58 C59 C11 -1.1(6) . . . . ?
N5 C11 C59 C58 1.0(6) . . . . ?
C32 C11 C59 C58 -176.6(4) . . . . ?
C48 N2 C62 C46 0.1(6) . . . . ?
C27 C46 C62 N2 1.1(6) . . . . ?
C33 N6 C63 C41 -0.9(5) . . . . ?
C33 N6 C63 C66 177.8(3) . . . . ?
C35 C41 C63 N6 1.3(5) . . . . ?
C35 C41 C63 C66 -177.3(3) . . . . ?
C71 C34 C64 C29 -0.4(6) . . . . ?
C25 C29 C64 C34 -0.7(6) . . . . ?
C32 N4 C66 C63 -148.0(3) . . . . ?
C17 N4 C66 C63 88.0(4) . . . . ?
N6 C63 C66 N4 40.6(4) . . . . ?
C41 C63 C66 N4 -140.7(3) . . . . ?
N5 C56 C68 C58 0.1(6) . . . . ?
C59 C58 C68 C56 0.6(6) . . . . ?
C25 N3 C71 C34 -0.4(6) . . . . ?
C64 C34 C71 N3 1.1(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        26.32
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.091
####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_r2677z
_database_code_depnum_ccdc_archive 'CCDC 1444963'
_audit_update_record             
;
2015-12-31 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Mn2(LCl-O)(mu-OAc)2](ClO4)(H2O)'
_chemical_formula_moiety         'C36 H36 Cl Mn2 N6 O5, Cl O4, O'
_chemical_formula_sum            'C36 H36 Cl2 Mn2 N6 O10'
_chemical_formula_weight         893.49

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'
Mn Mn 0.3368 0.7283 '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/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   10.2227(2)
_cell_length_b                   13.9012(4)
_cell_length_c                   28.2107(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4990(10)
_cell_angle_gamma                90.00
_cell_volume                     4007.59(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9094
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      30.00

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1832
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7722
_exptl_absorpt_correction_T_max  0.9220
_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       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            111141
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         29.00
_reflns_number_total             10643
_reflns_number_gt                9734
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0343P)²+3.9767P] 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         10643
_refine_ls_number_parameters     525
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0798
_refine_ls_wR_factor_gt          0.0777
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.002
_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
Mn2 Mn 0.75077(2) 0.373790(15) 0.397675(7) 0.01114(5) Uani 1 1 d . . .
Mn1 Mn 0.43105(2) 0.305616(15) 0.415301(7) 0.01123(5) Uani 1 1 d . . .
Cl2 Cl 0.12034(3) 0.87957(2) 0.346989(12) 0.01586(7) Uani 1 1 d . . .
Cl1 Cl 0.50978(4) 0.17866(3) 0.169031(13) 0.02294(8) Uani 1 1 d . . .
O1 O 0.58229(10) 0.30957(7) 0.36559(3) 0.01264(19) Uani 1 1 d . . .
O2 O 0.44519(10) 0.44683(8) 0.44037(4) 0.0169(2) Uani 1 1 d . . .
O4 O 0.56015(10) 0.22738(8) 0.46448(4) 0.0178(2) Uani 1 1 d . . .
O5 O 0.75699(11) 0.29717(9) 0.46170(4) 0.0208(2) Uani 1 1 d . . .
O7 O 0.08482(13) 0.91633(10) 0.39272(4) 0.0272(3) Uani 1 1 d . . .
O9 O 0.18432(13) 0.95484(8) 0.32074(4) 0.0245(3) Uani 1 1 d . . .
O3 O 0.64386(11) 0.49774(8) 0.42011(4) 0.0206(2) Uani 1 1 d . . .
O8 O 0.20785(13) 0.79940(9) 0.35319(5) 0.0313(3) Uani 1 1 d . . .
O6 O 0.00413(13) 0.84940(11) 0.32101(5) 0.0326(3) Uani 1 1 d . . .
N6 N 0.86312(12) 0.25563(9) 0.35877(4) 0.0144(2) Uani 1 1 d . . .
N4 N 0.78719(11) 0.43565(8) 0.32220(4) 0.0108(2) Uani 1 1 d . . .
N2 N 0.27152(12) 0.24550(9) 0.46009(4) 0.0160(2) Uani 1 1 d . . .
N3 N 0.29816(12) 0.35803(9) 0.35200(4) 0.0136(2) Uani 1 1 d . . .
N5 N 0.92879(12) 0.47130(9) 0.40373(4) 0.0140(2) Uani 1 1 d . . .
N1 N 0.35948(12) 0.16698(9) 0.37667(4) 0.0139(2) Uani 1 1 d . . .
C6 C 0.60983(13) 0.33719(10) 0.28314(5) 0.0115(2) Uani 1 1 d . . .
C5 C 0.59196(14) 0.30577(10) 0.23641(5) 0.0135(3) Uani 1 1 d . . .
H5 H 0.6175 0.3454 0.2108 0.016 Uiso 1 1 calc R . .
C22 C 0.93570(13) 0.53885(10) 0.36955(5) 0.0127(3) Uani 1 1 d . . .
C20 C 0.66398(13) 0.43620(10) 0.29303(5) 0.0117(2) Uani 1 1 d . . .
H20A H 0.6805 0.4685 0.2625 0.014 Uiso 1 1 calc R . .
H20B H 0.5975 0.4743 0.3097 0.014 Uiso 1 1 calc R . .
C23 C 1.03244(14) 0.60927(10) 0.37036(6) 0.0163(3) Uani 1 1 d . . .
H23 H 1.0354 0.6562 0.3459 0.020 Uiso 1 1 calc R . .
C28 C 0.88836(13) 0.27439(10) 0.31320(5) 0.0129(3) Uani 1 1 d . . .
C33 C 0.53031(14) 0.51165(10) 0.43459(5) 0.0132(3) Uani 1 1 d . . .
C1 C 0.57032(13) 0.27848(10) 0.32109(5) 0.0111(2) Uani 1 1 d . . .
C2 C 0.51580(14) 0.18712(10) 0.31117(5) 0.0134(3) Uani 1 1 d . . .
C15 C 0.25986(13) 0.28736(11) 0.32210(5) 0.0141(3) Uani 1 1 d . . .
C3 C 0.50029(14) 0.15658(11) 0.26434(5) 0.0156(3) Uani 1 1 d . . .
H3 H 0.4648 0.0948 0.2576 0.019 Uiso 1 1 calc R . .
C21 C 0.83083(14) 0.53529(10) 0.33092(5) 0.0132(3) Uani 1 1 d . . .
H21A H 0.7553 0.5749 0.3403 0.016 Uiso 1 1 calc R . .
H21B H 0.8654 0.5626 0.3014 0.016 Uiso 1 1 calc R . .
C19 C 0.30599(14) 0.44806(11) 0.33489(5) 0.0163(3) Uani 1 1 d . . .
H19 H 0.3330 0.4981 0.3559 0.020 Uiso 1 1 calc R . .
C27 C 0.89105(14) 0.37926(10) 0.29916(5) 0.0130(3) Uani 1 1 d . . .
H27A H 0.9775 0.4068 0.3081 0.016 Uiso 1 1 calc R . .
H27B H 0.8795 0.3845 0.2643 0.016 Uiso 1 1 calc R . .
C29 C 0.91805(14) 0.20199(11) 0.28097(6) 0.0174(3) Uani 1 1 d . . .
H29 H 0.9347 0.2171 0.2488 0.021 Uiso 1 1 calc R . .
C4 C 0.53658(14) 0.21622(11) 0.22763(5) 0.0154(3) Uani 1 1 d . . .
C16 C 0.22961(14) 0.30479(11) 0.27444(5) 0.0173(3) Uani 1 1 d . . .
H16 H 0.2035 0.2535 0.2540 0.021 Uiso 1 1 calc R . .
C17 C 0.23808(15) 0.39793(12) 0.25712(6) 0.0199(3) Uani 1 1 d . . .
H17 H 0.2180 0.4114 0.2247 0.024 Uiso 1 1 calc R . .
C24 C 1.12473(15) 0.60990(11) 0.40744(6) 0.0194(3) Uani 1 1 d . . .
H24 H 1.1909 0.6578 0.4089 0.023 Uiso 1 1 calc R . .
C34 C 0.49083(16) 0.61332(11) 0.44636(5) 0.0186(3) Uani 1 1 d . . .
H34A H 0.5613 0.6576 0.4381 0.028 Uiso 1 1 calc R . .
H34B H 0.4746 0.6182 0.4804 0.028 Uiso 1 1 calc R . .
H34C H 0.4110 0.6302 0.4283 0.028 Uiso 1 1 calc R . .
C13 C 0.21384(16) 0.29102(13) 0.49600(6) 0.0215(3) Uani 1 1 d . . .
H13 H 0.2344 0.3568 0.5016 0.026 Uiso 1 1 calc R . .
C9 C 0.24152(14) 0.15282(11) 0.45177(6) 0.0177(3) Uani 1 1 d . . .
C7 C 0.47139(15) 0.12394(10) 0.35114(5) 0.0150(3) Uani 1 1 d . . .
H7A H 0.4448 0.0605 0.3382 0.018 Uiso 1 1 calc R . .
H7B H 0.5455 0.1136 0.3739 0.018 Uiso 1 1 calc R . .
C8 C 0.31831(16) 0.10070(11) 0.41456(6) 0.0187(3) Uani 1 1 d . . .
H8A H 0.3967 0.0707 0.4297 0.022 Uiso 1 1 calc R . .
H8B H 0.2637 0.0488 0.4004 0.022 Uiso 1 1 calc R . .
C18 C 0.27643(15) 0.47121(11) 0.28805(6) 0.0193(3) Uani 1 1 d . . .
H18 H 0.2822 0.5358 0.2773 0.023 Uiso 1 1 calc R . .
C14 C 0.24787(14) 0.18884(11) 0.34400(5) 0.0164(3) Uani 1 1 d . . .
H14A H 0.1655 0.1853 0.3616 0.020 Uiso 1 1 calc R . .
H14B H 0.2436 0.1399 0.3185 0.020 Uiso 1 1 calc R . .
C35 C 0.67736(15) 0.23734(11) 0.47821(5) 0.0161(3) Uani 1 1 d . . .
C30 C 0.92280(15) 0.10752(11) 0.29669(6) 0.0213(3) Uani 1 1 d . . .
H30 H 0.9444 0.0571 0.2756 0.026 Uiso 1 1 calc R . .
C25 C 1.11906(15) 0.53966(12) 0.44232(6) 0.0203(3) Uani 1 1 d . . .
H25 H 1.1817 0.5381 0.4678 0.024 Uiso 1 1 calc R . .
C26 C 1.01966(15) 0.47188(11) 0.43906(5) 0.0178(3) Uani 1 1 d . . .
H26 H 1.0156 0.4237 0.4629 0.021 Uiso 1 1 calc R . .
C31 C 0.89561(16) 0.08750(11) 0.34362(6) 0.0226(3) Uani 1 1 d . . .
H31 H 0.8975 0.0233 0.3551 0.027 Uiso 1 1 calc R . .
C32 C 0.86569(15) 0.16313(11) 0.37329(6) 0.0191(3) Uani 1 1 d . . .
H32 H 0.8461 0.1494 0.4053 0.023 Uiso 1 1 calc R . .
C12 C 0.12578(18) 0.24603(15) 0.52510(7) 0.0310(4) Uani 1 1 d . . .
H12 H 0.0880 0.2797 0.5507 0.037 Uiso 1 1 calc R . .
C10 C 0.15034(17) 0.10378(13) 0.47866(7) 0.0278(4) Uani 1 1 d . . .
H10 H 0.1274 0.0391 0.4713 0.033 Uiso 1 1 calc R . .
C11 C 0.09381(19) 0.15087(15) 0.51621(8) 0.0353(5) Uani 1 1 d . . .
H11 H 0.0337 0.1182 0.5357 0.042 Uiso 1 1 calc R . .
C36 C 0.7265(2) 0.17342(17) 0.51806(8) 0.0387(5) Uani 1 1 d . . .
H36A H 0.7253 0.1062 0.5075 0.058 Uiso 1 1 calc R . .
H36B H 0.6701 0.1807 0.5454 0.058 Uiso 1 1 calc R . .
H36C H 0.8163 0.1918 0.5272 0.058 Uiso 1 1 calc R . .
O10 O 0.4595(4) 0.0698(3) 0.51944(15) 0.0597(11) Uani 0.48 1 d P A 1
O11 O 0.4164(5) 0.0994(4) 0.5720(2) 0.0525(15) Uani 0.30 1 d PU B 2
O12 O 0.3727(8) 0.0142(6) 0.5587(3) 0.058(2) Uani 0.22 1 d PU C 3


_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
Mn2 O5 2.0964(11) . ?
Mn2 O1 2.1216(10) . ?
Mn2 O3 2.1448(11) . ?
Mn2 N5 2.2721(12) . ?
Mn2 N6 2.2995(12) . ?
Mn2 N4 2.3352(12) . ?
Mn1 O2 2.0903(11) . ?
Mn1 O1 2.1150(10) . ?
Mn1 O4 2.1803(11) . ?
Mn1 N2 2.2499(12) . ?
Mn1 N1 2.3228(13) . ?
Mn1 N3 2.3319(12) . ?
Cl2 O8 1.4370(12) . ?
Cl2 O6 1.4418(13) . ?
Cl2 O7 1.4427(12) . ?
Cl2 O9 1.4479(11) . ?
Cl1 C4 1.7484(15) . ?
O1 C1 1.3303(16) . ?
O2 C33 1.2660(18) . ?
O4 C35 1.2571(19) . ?
O5 C35 1.2615(19) . ?
O3 C33 1.2556(18) . ?
N6 C28 1.3432(19) . ?
N6 C32 1.3495(19) . ?
N4 C21 1.4739(17) . ?
N4 C27 1.4834(17) . ?
N4 C20 1.4864(17) . ?
N2 C13 1.344(2) . ?
N2 C9 1.344(2) . ?
N3 C19 1.3446(19) . ?
N3 C15 1.3464(19) . ?
N5 C26 1.3446(19) . ?
N5 C22 1.3491(18) . ?
N1 C14 1.4794(19) . ?
N1 C8 1.4806(18) . ?
N1 C7 1.4929(18) . ?
C6 C5 1.3962(19) . ?
C6 C1 1.4134(19) . ?
C6 C20 1.5069(19) . ?
C5 C4 1.387(2) . ?
C5 H5 0.9500 . ?
C22 C23 1.391(2) . ?
C22 C21 1.5094(19) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C23 C24 1.390(2) . ?
C23 H23 0.9500 . ?
C28 C29 1.395(2) . ?
C28 C27 1.5112(19) . ?
C33 C34 1.509(2) . ?
C1 C2 1.4120(19) . ?
C2 C3 1.393(2) . ?
C2 C7 1.5086(19) . ?
C15 C16 1.393(2) . ?
C15 C14 1.509(2) . ?
C3 C4 1.385(2) . ?
C3 H3 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C19 C18 1.386(2) . ?
C19 H19 0.9500 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C29 C30 1.387(2) . ?
C29 H29 0.9500 . ?
C16 C17 1.387(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(2) . ?
C17 H17 0.9500 . ?
C24 C25 1.388(2) . ?
C24 H24 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C13 C12 1.384(2) . ?
C13 H13 0.9500 . ?
C9 C10 1.395(2) . ?
C9 C8 1.512(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C18 H18 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C35 C36 1.509(2) . ?
C30 C31 1.388(2) . ?
C30 H30 0.9500 . ?
C25 C26 1.387(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C32 1.383(2) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C12 C11 1.384(3) . ?
C12 H12 0.9500 . ?
C10 C11 1.384(3) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 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
O5 Mn2 O1 99.19(4) . . ?
O5 Mn2 O3 99.10(5) . . ?
O1 Mn2 O3 92.84(4) . . ?
O5 Mn2 N5 103.43(4) . . ?
O1 Mn2 N5 157.35(4) . . ?
O3 Mn2 N5 84.94(4) . . ?
O5 Mn2 N6 92.52(5) . . ?
O1 Mn2 N6 84.60(4) . . ?
O3 Mn2 N6 168.35(5) . . ?
N5 Mn2 N6 93.04(4) . . ?
O5 Mn2 N4 166.10(4) . . ?
O1 Mn2 N4 85.01(4) . . ?
O3 Mn2 N4 93.89(4) . . ?
N5 Mn2 N4 72.69(4) . . ?
N6 Mn2 N4 74.59(4) . . ?
O2 Mn1 O1 98.89(4) . . ?
O2 Mn1 O4 102.58(4) . . ?
O1 Mn1 O4 89.66(4) . . ?
O2 Mn1 N2 101.74(5) . . ?
O1 Mn1 N2 159.26(4) . . ?
O4 Mn1 N2 83.85(4) . . ?
O2 Mn1 N1 162.95(4) . . ?
O1 Mn1 N1 86.40(4) . . ?
O4 Mn1 N1 93.60(4) . . ?
N2 Mn1 N1 74.41(5) . . ?
O2 Mn1 N3 89.96(4) . . ?
O1 Mn1 N3 84.58(4) . . ?
O4 Mn1 N3 166.89(4) . . ?
N2 Mn1 N3 97.46(4) . . ?
N1 Mn1 N3 74.33(4) . . ?
O8 Cl2 O6 109.77(9) . . ?
O8 Cl2 O7 109.65(8) . . ?
O6 Cl2 O7 109.53(8) . . ?
O8 Cl2 O9 109.54(7) . . ?
O6 Cl2 O9 109.11(8) . . ?
O7 Cl2 O9 109.21(8) . . ?
C1 O1 Mn1 124.51(8) . . ?
C1 O1 Mn2 126.36(8) . . ?
Mn1 O1 Mn2 109.11(4) . . ?
C33 O2 Mn1 131.80(9) . . ?
C35 O4 Mn1 134.22(10) . . ?
C35 O5 Mn2 130.38(10) . . ?
C33 O3 Mn2 134.61(10) . . ?
C28 N6 C32 118.21(13) . . ?
C28 N6 Mn2 115.40(9) . . ?
C32 N6 Mn2 122.80(10) . . ?
C21 N4 C27 110.65(11) . . ?
C21 N4 C20 109.63(11) . . ?
C27 N4 C20 111.47(11) . . ?
C21 N4 Mn2 104.40(8) . . ?
C27 N4 Mn2 109.75(8) . . ?
C20 N4 Mn2 110.71(8) . . ?
C13 N2 C9 118.73(13) . . ?
C13 N2 Mn1 125.97(11) . . ?
C9 N2 Mn1 115.05(10) . . ?
C19 N3 C15 118.24(13) . . ?
C19 N3 Mn1 121.79(10) . . ?
C15 N3 Mn1 113.95(9) . . ?
C26 N5 C22 118.53(13) . . ?
C26 N5 Mn2 126.57(10) . . ?
C22 N5 Mn2 114.73(9) . . ?
C14 N1 C8 110.39(11) . . ?
C14 N1 C7 111.72(11) . . ?
C8 N1 C7 109.56(11) . . ?
C14 N1 Mn1 110.50(9) . . ?
C8 N1 Mn1 105.64(9) . . ?
C7 N1 Mn1 108.84(8) . . ?
C5 C6 C1 120.10(13) . . ?
C5 C6 C20 119.92(12) . . ?
C1 C6 C20 119.87(12) . . ?
C4 C5 C6 119.48(13) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
N5 C22 C23 121.90(13) . . ?
N5 C22 C21 116.35(12) . . ?
C23 C22 C21 121.73(13) . . ?
N4 C20 C6 113.55(11) . . ?
N4 C20 H20A 108.9 . . ?
C6 C20 H20A 108.9 . . ?
N4 C20 H20B 108.9 . . ?
C6 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C24 C23 C22 119.00(14) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
N6 C28 C29 122.29(14) . . ?
N6 C28 C27 116.32(12) . . ?
C29 C28 C27 121.28(13) . . ?
O3 C33 O2 125.22(13) . . ?
O3 C33 C34 118.07(13) . . ?
O2 C33 C34 116.71(13) . . ?
O1 C1 C2 120.35(12) . . ?
O1 C1 C6 120.41(12) . . ?
C2 C1 C6 119.23(12) . . ?
C3 C2 C1 119.79(13) . . ?
C3 C2 C7 120.17(13) . . ?
C1 C2 C7 120.03(12) . . ?
N3 C15 C16 122.11(14) . . ?
N3 C15 C14 115.54(13) . . ?
C16 C15 C14 122.33(13) . . ?
C4 C3 C2 120.05(13) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
N4 C21 C22 110.94(11) . . ?
N4 C21 H21A 109.5 . . ?
C22 C21 H21A 109.5 . . ?
N4 C21 H21B 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 108.0 . . ?
N3 C19 C18 123.03(14) . . ?
N3 C19 H19 118.5 . . ?
C18 C19 H19 118.5 . . ?
N4 C27 C28 112.13(11) . . ?
N4 C27 H27A 109.2 . . ?
C28 C27 H27A 109.2 . . ?
N4 C27 H27B 109.2 . . ?
C28 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
C30 C29 C28 118.76(15) . . ?
C30 C29 H29 120.6 . . ?
C28 C29 H29 120.6 . . ?
C3 C4 C5 121.32(13) . . ?
C3 C4 Cl1 119.33(11) . . ?
C5 C4 Cl1 119.34(11) . . ?
C17 C16 C15 119.21(14) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C16 C17 C18 118.80(14) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
C25 C24 C23 119.26(14) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N2 C13 C12 122.65(17) . . ?
N2 C13 H13 118.7 . . ?
C12 C13 H13 118.7 . . ?
N2 C9 C10 121.75(15) . . ?
N2 C9 C8 117.42(13) . . ?
C10 C9 C8 120.65(15) . . ?
N1 C7 C2 112.13(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 . . ?
N1 C8 C9 111.44(12) . . ?
N1 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
N1 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C19 C18 C17 118.62(14) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
N1 C14 C15 111.83(11) . . ?
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 . . ?
O4 C35 O5 125.29(14) . . ?
O4 C35 C36 117.46(15) . . ?
O5 C35 C36 117.24(15) . . ?
C29 C30 C31 119.26(14) . . ?
C29 C30 H30 120.4 . . ?
C31 C30 H30 120.4 . . ?
C26 C25 C24 118.34(14) . . ?
C26 C25 H25 120.8 . . ?
C24 C25 H25 120.8 . . ?
N5 C26 C25 122.95(14) . . ?
N5 C26 H26 118.5 . . ?
C25 C26 H26 118.5 . . ?
C32 C31 C30 118.54(15) . . ?
C32 C31 H31 120.7 . . ?
C30 C31 H31 120.7 . . ?
N6 C32 C31 122.92(15) . . ?
N6 C32 H32 118.5 . . ?
C31 C32 H32 118.5 . . ?
C11 C12 C13 118.61(17) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C11 C10 C9 118.91(17) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C12 C11 C10 119.29(16) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 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 -0.7(2) . . . . ?
C20 C6 C5 C4 -177.12(13) . . . . ?
C26 N5 C22 C23 -1.0(2) . . . . ?
C26 N5 C22 C21 -179.63(13) . . . . ?
C21 N4 C20 C6 -178.68(11) . . . . ?
C27 N4 C20 C6 58.45(14) . . . . ?
C5 C6 C20 N4 -121.05(14) . . . . ?
C1 C6 C20 N4 62.54(16) . . . . ?
N5 C22 C23 C24 0.1(2) . . . . ?
C21 C22 C23 C24 178.67(14) . . . . ?
C32 N6 C28 C29 -0.6(2) . . . . ?
C32 N6 C28 C27 -177.04(13) . . . . ?
C5 C6 C1 O1 -177.32(12) . . . . ?
C20 C6 C1 O1 -0.92(19) . . . . ?
C5 C6 C1 C2 1.5(2) . . . . ?
C20 C6 C1 C2 177.94(12) . . . . ?
O1 C1 C2 C3 178.13(13) . . . . ?
C6 C1 C2 C3 -0.7(2) . . . . ?
O1 C1 C2 C7 -0.3(2) . . . . ?
C6 C1 C2 C7 -179.19(13) . . . . ?
C19 N3 C15 C16 0.5(2) . . . . ?
C19 N3 C15 C14 -177.61(12) . . . . ?
C1 C2 C3 C4 -0.9(2) . . . . ?
C7 C2 C3 C4 177.56(14) . . . . ?
C27 N4 C21 C22 -70.25(14) . . . . ?
C20 N4 C21 C22 166.40(11) . . . . ?
N5 C22 C21 N4 -31.35(17) . . . . ?
C23 C22 C21 N4 150.01(13) . . . . ?
C15 N3 C19 C18 0.0(2) . . . . ?
C21 N4 C27 C28 148.30(12) . . . . ?
C20 N4 C27 C28 -89.42(14) . . . . ?
N6 C28 C27 N4 -39.41(17) . . . . ?
C29 C28 C27 N4 144.14(13) . . . . ?
N6 C28 C29 C30 -0.6(2) . . . . ?
C27 C28 C29 C30 175.62(13) . . . . ?
C2 C3 C4 C5 1.8(2) . . . . ?
C2 C3 C4 Cl1 -177.25(11) . . . . ?
C6 C5 C4 C3 -0.9(2) . . . . ?
C6 C5 C4 Cl1 178.07(11) . . . . ?
N3 C15 C16 C17 -0.5(2) . . . . ?
C14 C15 C16 C17 177.52(14) . . . . ?
C15 C16 C17 C18 -0.1(2) . . . . ?
C22 C23 C24 C25 0.8(2) . . . . ?
C9 N2 C13 C12 0.7(2) . . . . ?
C13 N2 C9 C10 1.5(2) . . . . ?
C13 N2 C9 C8 -173.73(14) . . . . ?
C14 N1 C7 C2 55.91(15) . . . . ?
C8 N1 C7 C2 178.56(12) . . . . ?
C3 C2 C7 N1 -113.61(15) . . . . ?
C1 C2 C7 N1 64.83(17) . . . . ?
C14 N1 C8 C9 -76.80(15) . . . . ?
C7 N1 C8 C9 159.76(12) . . . . ?
N2 C9 C8 N1 -31.20(19) . . . . ?
C10 C9 C8 N1 153.55(15) . . . . ?
N3 C19 C18 C17 -0.6(2) . . . . ?
C16 C17 C18 C19 0.7(2) . . . . ?
C8 N1 C14 C15 150.67(12) . . . . ?
C7 N1 C14 C15 -87.15(14) . . . . ?
N3 C15 C14 N1 -43.47(17) . . . . ?
C16 C15 C14 N1 138.37(14) . . . . ?
C28 C29 C30 C31 1.2(2) . . . . ?
C23 C24 C25 C26 -0.8(2) . . . . ?
C22 N5 C26 C25 1.0(2) . . . . ?
C24 C25 C26 N5 -0.1(2) . . . . ?
C29 C30 C31 C32 -0.6(2) . . . . ?
C28 N6 C32 C31 1.3(2) . . . . ?
C30 C31 C32 N6 -0.7(2) . . . . ?
N2 C13 C12 C11 -1.4(3) . . . . ?
N2 C9 C10 C11 -2.9(3) . . . . ?
C8 C9 C10 C11 172.15(17) . . . . ?
C13 C12 C11 C10 -0.1(3) . . . . ?
C9 C10 C11 C12 2.1(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.062
