# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_1_DBL7
_database_code_depnum_ccdc_archive 'CCDC 1005503'
_audit_update_record             
;
2014-05-27 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_formula_moiety         '2(C18 H25 N2 Ni0.5 O)'
_chemical_formula_sum            'C36 H50 N4 Ni O2'
_chemical_formula_weight         629.51
_chemical_melting_point          ?
_chemical_name_common            ?
_chemical_name_systematic        ?
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'
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 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_angle_alpha                90.00
_cell_angle_beta                 92.410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.3610(6)
_cell_length_b                   10.3225(4)
_cell_length_c                   9.2567(3)
_cell_measurement_reflns_used    4682
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      28.871
_cell_measurement_theta_min      2.296
_cell_volume                     1657.42(10)
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.4055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 SADABS-2006/1 (Bruker,2006) was used for absorption correction.
 R(int) was 0.0477 before and 0.0315 after correction.
 The Ratio of minimum to maximum transmission is 0.4055.
 The λ/2 correction factor is 0.0015
;
_exptl_crystal_F_000             676
_exptl_crystal_colour            green
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 The data collection nominally covered a full sphere of reciprocal space by
 a combination of 4 sets of ω scans each set at different φ and/or
 2θ angles and each scan (15.00 s exposure) covering -0.300\ degrees in ω.
 The crystal to detector distance was 4.85 cm.
;
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19777
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.30
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           5.0
_diffrn_source_power             0.1
_diffrn_source_target            MO
_diffrn_source_voltage           20.0
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3393
_reflns_number_total             4400
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    
;
OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material  
;
OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    
;
A short history of SHELX (Sheldrick, 2007)/Bruker
;
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.075
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0448
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1261
_refine_ls_weighting_details     
;
calc w=1/[σ²(Fo²)+(0.0600P)²+1.7000P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_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. 
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.5000 0.5000 0.01751(11) Uani 1 2 d S . .
O1 O 0.10204(8) 0.50634(13) 0.44360(15) 0.0193(3) Uani 1 1 d . . .
N1 N 0.03209(9) 0.44750(16) 0.68393(18) 0.0193(3) Uani 1 1 d . . .
N2 N -0.01945(9) 0.41758(16) 0.78448(18) 0.0202(3) Uani 1 1 d . . .
C1 C 0.01423(11) 0.35939(19) 0.9001(2) 0.0214(4) Uani 1 1 d . . .
C2 C 0.09177(12) 0.35058(19) 0.8742(2) 0.0216(4) Uani 1 1 d . . .
C3 C 0.10115(11) 0.40829(18) 0.7371(2) 0.0195(4) Uani 1 1 d . . .
C4 C 0.17135(11) 0.43289(18) 0.6603(2) 0.0201(4) Uani 1 1 d . . .
C5 C 0.16821(11) 0.48541(18) 0.5182(2) 0.0190(4) Uani 1 1 d . . .
C6 C 0.24007(11) 0.51451(19) 0.4547(2) 0.0206(4) Uani 1 1 d . . .
C7 C 0.30799(12) 0.4912(2) 0.5348(2) 0.0229(4) Uani 1 1 d . . .
C8 C 0.31168(11) 0.4391(2) 0.6744(2) 0.0238(4) Uani 1 1 d . A .
C9 C 0.24212(11) 0.4101(2) 0.7342(2) 0.0228(4) Uani 1 1 d . . .
C10 C 0.38858(11) 0.4175(2) 0.7586(2) 0.0283(5) Uani 1 1 d . . .
C11 C 0.3863(2) 0.4943(4) 0.9012(4) 0.0339(8) Uiso 0.60 1 d P A 1
H11B H 0.3784 0.5864 0.8797 0.051 Uiso 0.60 1 calc PR A 1
H11C H 0.4351 0.4829 0.9566 0.051 Uiso 0.60 1 calc PR A 1
H11A H 0.3438 0.4624 0.9579 0.051 Uiso 0.60 1 calc PR A 1
C11A C 0.4306(5) 0.5411(8) 0.7834(9) 0.0501(17) Uiso 0.40 1 d P A 2
H11D H 0.4349 0.5868 0.6912 0.075 Uiso 0.40 1 calc PR A 2
H11F H 0.4823 0.5230 0.8251 0.075 Uiso 0.40 1 calc PR A 2
H11E H 0.4025 0.5953 0.8502 0.075 Uiso 0.40 1 calc PR A 2
C12 C 0.4576(3) 0.4678(4) 0.6768(5) 0.0374(9) Uiso 0.60 1 d P A 1
H12A H 0.4625 0.4175 0.5878 0.056 Uiso 0.60 1 calc PR A 1
H12C H 0.5048 0.4585 0.7379 0.056 Uiso 0.60 1 calc PR A 1
H12B H 0.4496 0.5593 0.6524 0.056 Uiso 0.60 1 calc PR A 1
C12A C 0.4402(4) 0.3243(7) 0.6693(7) 0.0415(14) Uiso 0.40 1 d P A 2
H12D H 0.4144 0.2404 0.6569 0.062 Uiso 0.40 1 calc PR A 2
H12F H 0.4901 0.3120 0.7211 0.062 Uiso 0.40 1 calc PR A 2
H12E H 0.4485 0.3625 0.5742 0.062 Uiso 0.40 1 calc PR A 2
C13 C 0.3983(3) 0.2762(5) 0.7907(5) 0.0453(10) Uiso 0.60 1 d P A 1
H13B H 0.3556 0.2464 0.8483 0.068 Uiso 0.60 1 calc PR A 1
H13C H 0.4472 0.2623 0.8450 0.068 Uiso 0.60 1 calc PR A 1
H13A H 0.3983 0.2276 0.6998 0.068 Uiso 0.60 1 calc PR A 1
C13A C 0.3808(4) 0.3449(7) 0.9070(7) 0.0415(14) Uiso 0.40 1 d P A 2
H13E H 0.3485 0.3961 0.9698 0.062 Uiso 0.40 1 calc PR A 2
H13F H 0.4320 0.3336 0.9538 0.062 Uiso 0.40 1 calc PR A 2
H13D H 0.3571 0.2599 0.8895 0.062 Uiso 0.40 1 calc PR A 2
C14 C 0.24286(11) 0.5715(2) 0.3007(2) 0.0244(4) Uani 1 1 d . . .
C15 C 0.20204(13) 0.7041(2) 0.2932(3) 0.0296(5) Uani 1 1 d . . .
C16 C 0.32603(13) 0.5966(3) 0.2560(3) 0.0327(5) Uani 1 1 d . . .
C17 C 0.20763(13) 0.4748(2) 0.1908(2) 0.0283(5) Uani 1 1 d . . .
C18 C -0.03196(13) 0.3194(2) 1.0247(2) 0.0252(4) Uani 1 1 d . . .
H2A H 0.1274(14) 0.313(2) 0.931(3) 0.025(6) Uiso 1 1 d . . .
H2 H -0.0646(16) 0.437(3) 0.767(3) 0.026(6) Uiso 1 1 d . . .
H7 H 0.3514(14) 0.511(2) 0.496(3) 0.016(6) Uiso 1 1 d . . .
H9 H 0.2412(15) 0.377(3) 0.829(3) 0.031(7) Uiso 1 1 d . . .
H15A H 0.1479(16) 0.701(3) 0.326(3) 0.036(7) Uiso 1 1 d . . .
H15B H 0.1992(15) 0.735(3) 0.190(3) 0.035(7) Uiso 1 1 d . . .
H15C H 0.2306(16) 0.766(3) 0.355(3) 0.036(7) Uiso 1 1 d . . .
H16A H 0.3552(17) 0.514(3) 0.256(3) 0.031(7) Uiso 1 1 d . . .
H16B H 0.3245(16) 0.633(3) 0.161(3) 0.037(7) Uiso 1 1 d . . .
H16C H 0.3524(18) 0.663(3) 0.317(3) 0.048(9) Uiso 1 1 d . . .
H17A H 0.1568(17) 0.447(3) 0.214(3) 0.036(7) Uiso 1 1 d . . .
H17B H 0.2403(16) 0.406(3) 0.181(3) 0.036(7) Uiso 1 1 d . . .
H17C H 0.2002(18) 0.515(3) 0.095(3) 0.039(8) Uiso 1 1 d . . .
H18B H -0.0666(15) 0.385(3) 1.049(3) 0.029(7) Uiso 1 1 d . . .
H18C H 0.0016(16) 0.303(3) 1.112(3) 0.041(8) Uiso 1 1 d . . .
H18A H -0.0619(13) 0.240(2) 1.003(2) 0.019(6) Uiso 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.8689(13) . ?
Ni1 O1 1.8689(13) 3_566 ?
Ni1 N1 1.8501(17) 3_566 ?
Ni1 N1 1.8501(17) . ?
O1 C5 1.333(2) . ?
N1 N2 1.354(2) . ?
N1 C3 1.339(2) . ?
N2 C1 1.340(3) . ?
N2 H2 0.82(3) . ?
C1 C2 1.380(3) . ?
C1 C18 1.490(3) . ?
C2 C3 1.417(3) . ?
C2 H2A 0.89(3) . ?
C3 C4 1.459(3) . ?
C4 C5 1.421(3) . ?
C4 C9 1.401(3) . ?
C5 C6 1.433(3) . ?
C6 C7 1.387(3) . ?
C6 C14 1.545(3) . ?
C7 C8 1.398(3) . ?
C7 H7 0.87(2) . ?
C8 C9 1.382(3) . ?
C8 C10 1.534(3) . ?
C9 H9 0.94(3) . ?
C10 C11 1.542(5) . ?
C10 C11A 1.483(8) . ?
C10 C12 1.534(5) . ?
C10 C12A 1.574(7) . ?
C10 C13 1.496(5) . ?
C10 C13A 1.576(7) . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11 H11A 0.9800 . ?
C11A H11D 0.9800 . ?
C11A H11F 0.9800 . ?
C11A H11E 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12C 0.9800 . ?
C12 H12B 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12F 0.9800 . ?
C12A H12E 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13 H13A 0.9800 . ?
C13A H13E 0.9800 . ?
C13A H13F 0.9800 . ?
C13A H13D 0.9800 . ?
C14 C15 1.542(3) . ?
C14 C16 1.540(3) . ?
C14 C17 1.534(3) . ?
C15 H15A 1.00(3) . ?
C15 H15B 1.01(3) . ?
C15 H15C 0.98(3) . ?
C16 H16A 1.00(3) . ?
C16 H16B 0.95(3) . ?
C16 H16C 0.99(3) . ?
C17 H17A 0.96(3) . ?
C17 H17B 0.92(3) . ?
C17 H17C 0.98(3) . ?
C18 H18B 0.94(3) . ?
C18 H18C 0.99(3) . ?
C18 H18A 0.99(2) . ?

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 O1 180.0 . 3_566 ?
O1 C5 C4 122.67(17) . . ?
O1 C5 C6 119.99(17) . . ?
N1 Ni1 O1 89.13(7) . 3_566 ?
N1 Ni1 O1 89.14(7) 3_566 . ?
N1 Ni1 O1 90.86(7) 3_566 3_566 ?
N1 Ni1 O1 90.87(7) . . ?
N1 Ni1 N1 180.00(4) 3_566 . ?
N1 N2 H2 117.4(18) . . ?
N1 C3 C2 108.73(17) . . ?
N1 C3 C4 121.42(17) . . ?
N2 N1 Ni1 121.16(13) . . ?
N2 C1 C2 106.65(17) . . ?
N2 C1 C18 120.74(18) . . ?
C1 N2 N1 111.89(16) . . ?
C1 N2 H2 130.7(18) . . ?
C1 C2 C3 106.13(17) . . ?
C1 C2 H2A 125.9(16) . . ?
C1 C18 H18B 111.1(16) . . ?
C1 C18 H18C 111.3(16) . . ?
C1 C18 H18A 111.7(13) . . ?
C2 C1 C18 132.60(19) . . ?
C2 C3 C4 129.75(18) . . ?
C3 N1 Ni1 131.06(13) . . ?
C3 N1 N2 106.60(16) . . ?
C3 C2 H2A 127.9(16) . . ?
C4 C5 C6 117.33(18) . . ?
C4 C9 H9 117.8(16) . . ?
C5 O1 Ni1 131.00(13) . . ?
C5 C4 C3 121.15(17) . . ?
C5 C6 C14 121.31(17) . . ?
C6 C7 C8 124.42(19) . . ?
C6 C7 H7 118.0(16) . . ?
C7 C6 C5 118.67(18) . . ?
C7 C6 C14 120.02(17) . . ?
C7 C8 C10 122.04(18) . . ?
C8 C7 H7 117.6(16) . . ?
C8 C9 C4 122.1(2) . . ?
C8 C9 H9 120.1(16) . . ?
C8 C10 C11 107.9(2) . . ?
C8 C10 C12 112.4(2) . . ?
C8 C10 C12A 109.0(3) . . ?
C8 C10 C13A 114.0(3) . . ?
C9 C4 C3 117.76(18) . . ?
C9 C4 C5 120.99(18) . . ?
C9 C8 C7 116.53(19) . . ?
C9 C8 C10 121.42(19) . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11A H11D 109.5 . . ?
C10 C11A H11F 109.5 . . ?
C10 C11A H11E 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12C 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12A H12D 109.5 . . ?
C10 C12A H12F 109.5 . . ?
C10 C12A H12E 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13A H13E 109.5 . . ?
C10 C13A H13F 109.5 . . ?
C10 C13A H13D 109.5 . . ?
C11 C10 C12A 143.1(3) . . ?
C11 C10 C13A 59.5(3) . . ?
C11A C10 C8 111.5(4) . . ?
C11A C10 C11 57.0(4) . . ?
C11A C10 C12 52.8(4) . . ?
C11A C10 C12A 108.6(4) . . ?
C11A C10 C13 139.2(4) . . ?
C11A C10 C13A 109.5(4) . . ?
H11D C11A H11F 109.5 . . ?
H11D C11A H11E 109.5 . . ?
H11F C11A H11E 109.5 . . ?
C12 C10 C11 107.3(3) . . ?
C12 C10 C12A 58.2(3) . . ?
C12 C10 C13A 133.5(3) . . ?
C12A C10 C13A 103.8(4) . . ?
H12D C12A H12F 109.5 . . ?
H12D C12A H12E 109.5 . . ?
H12F C12A H12E 109.5 . . ?
C13 C10 C8 109.3(2) . . ?
C13 C10 C11 109.7(3) . . ?
C13 C10 C12 110.1(3) . . ?
C13 C10 C12A 56.4(3) . . ?
C13 C10 C13A 51.4(3) . . ?
H13E C13A H13F 109.5 . . ?
H13E C13A H13D 109.5 . . ?
H13F C13A H13D 109.5 . . ?
C14 C15 H15A 113.0(16) . . ?
C14 C15 H15B 109.2(16) . . ?
C14 C15 H15C 109.6(16) . . ?
C14 C16 H16A 109.8(16) . . ?
C14 C16 H16B 108.9(17) . . ?
C14 C16 H16C 112.4(18) . . ?
C14 C17 H17A 112.8(17) . . ?
C14 C17 H17B 109.9(18) . . ?
C14 C17 H17C 111.0(17) . . ?
C15 C14 C6 110.31(17) . . ?
C16 C14 C6 112.19(18) . . ?
C16 C14 C15 105.82(18) . . ?
C17 C14 C6 109.73(17) . . ?
C17 C14 C15 112.22(18) . . ?
C17 C14 C16 106.50(18) . . ?
H15A C15 H15B 107(2) . . ?
H15A C15 H15C 108(2) . . ?
H15B C15 H15C 110(2) . . ?
H16A C16 H16B 109(2) . . ?
H16A C16 H16C 112(2) . . ?
H16B C16 H16C 104(2) . . ?
H17A C17 H17B 112(2) . . ?
H17A C17 H17C 104(2) . . ?
H17B C17 H17C 107(2) . . ?
H18B C18 H18C 106(2) . . ?
H18B C18 H18A 108(2) . . ?
H18C C18 H18A 108(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 O1 0.82(3) 2.11(3) 2.622(2) 121(2) 3_566
####################################################################### 
# 
# 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_2_lb2
_database_code_depnum_ccdc_archive 'CCDC 1005504'
_audit_update_record             
;
2014-05-27 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56.40 H79.80 Cl4.80 F12 N6 Ni O3 Sb2'
_chemical_formula_sum            'C56.40 H79.80 Cl4.80 F12 N6 Ni O3 Sb2'
_chemical_formula_weight         1590.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.0749(6)
_cell_length_b                   15.0749(6)
_cell_length_c                   54.398(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10705.9(9)
_cell_formula_units_Z            6
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    206
_cell_measurement_theta_min      1.123
_cell_measurement_theta_max      26.368

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_F_000             4822.8
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.084
_exptl_absorpt_coefficient_mu    1.266
_shelx_estimated_absorpt_T_min   0.793
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '0.5 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_reflns_number            18973
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.123
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4873
_reflns_number_gt                4350
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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     
'w=1/[σ²(Fo²)+(0.0285P)²+141.3820P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4873
_refine_ls_number_parameters     269
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0468
_refine_ls_wR_factor_ref         0.1178
_refine_ls_wR_factor_gt          0.1115
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_restrained_S_all      1.345
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.6667 0.3333 0.43698(2) 0.01455(19) Uani 1 3 d S T P . .
N2 N 0.6022(2) 0.4081(2) 0.45424(6) 0.0163(7) Uani 1 1 d . . . . .
N3 N 0.6481(3) 0.4750(3) 0.47306(6) 0.0191(7) Uani 1 1 d . . . . .
H3 H 0.6949 0.4748 0.4827 0.023 Uiso 1 1 calc R U . . .
C4 C 0.6137(3) 0.5414(3) 0.47533(8) 0.0224(9) Uani 1 1 d . . . . .
C5 C 0.6525(4) 0.6216(4) 0.49499(9) 0.0323(11) Uani 1 1 d . . . . .
H5A H 0.7170 0.6809 0.4896 0.048 Uiso 1 1 calc R U . . .
H5B H 0.6640 0.5935 0.5101 0.048 Uiso 1 1 calc R U . . .
H5C H 0.6018 0.6429 0.4981 0.048 Uiso 1 1 calc R U . . .
C6 C 0.5436(3) 0.5183(3) 0.45702(8) 0.0224(9) Uani 1 1 d . . . . .
H6 H 0.5061 0.5521 0.4537 0.027 Uiso 1 1 calc R U . . .
C7 C 0.5377(3) 0.4347(3) 0.44404(7) 0.0167(8) Uani 1 1 d . . . . .
C8 C 0.4739(3) 0.3841(3) 0.42257(7) 0.0166(8) Uani 1 1 d . . . . .
C9 C 0.4788(3) 0.3026(3) 0.40920(7) 0.0156(8) Uani 1 1 d . . . . .
O10 O 0.5422(2) 0.2748(2) 0.41481(5) 0.0168(5) Uani 1 1 d . . . . .
C11 C 0.4081(3) 0.2524(3) 0.38860(7) 0.0160(8) Uani 1 1 d . . . . .
C12 C 0.4088(3) 0.1630(3) 0.37536(7) 0.0194(8) Uani 1 1 d . . . . .
C13 C 0.3328(3) 0.1232(3) 0.35378(8) 0.0273(10) Uani 1 1 d . . . . .
H13A H 0.3492 0.1794 0.3423 0.041 Uiso 1 1 calc R U . . .
H13B H 0.2630 0.0963 0.3600 0.041 Uiso 1 1 calc R U . . .
H13C H 0.3377 0.0685 0.3453 0.041 Uiso 1 1 calc R U . . .
C14 C 0.3768(3) 0.0739(3) 0.39349(9) 0.0269(9) Uani 1 1 d . . . . .
H14A H 0.3775 0.0167 0.3851 0.040 Uiso 1 1 calc R U . . .
H14B H 0.3077 0.0516 0.3996 0.040 Uiso 1 1 calc R U . . .
H14C H 0.4250 0.0966 0.4073 0.040 Uiso 1 1 calc R U . . .
C15 C 0.5161(3) 0.1966(3) 0.36470(8) 0.0236(9) Uani 1 1 d . . . . .
H15A H 0.5149 0.1384 0.3563 0.035 Uiso 1 1 calc R U . . .
H15B H 0.5664 0.2201 0.3781 0.035 Uiso 1 1 calc R U . . .
H15C H 0.5350 0.2525 0.3529 0.035 Uiso 1 1 calc R U . . .
C16 C 0.3442(3) 0.2881(3) 0.38187(7) 0.0190(8) Uani 1 1 d . . . . .
H16 H 0.2988 0.2562 0.3685 0.023 Uiso 1 1 calc R U . . .
C17 C 0.3426(3) 0.3702(3) 0.39390(7) 0.0189(8) Uani 1 1 d . . . . .
C18 C 0.2751(3) 0.4133(3) 0.38565(8) 0.0221(9) Uani 1 1 d . . . . .
C19 C 0.2123(4) 0.3606(4) 0.36265(9) 0.0291(10) Uani 1 1 d . . . . .
H19A H 0.1735 0.3939 0.3577 0.044 Uiso 1 1 calc R U . . .
H19B H 0.1647 0.2882 0.3663 0.044 Uiso 1 1 calc R U . . .
H19C H 0.2584 0.3659 0.3493 0.044 Uiso 1 1 calc R U . . .
C20 C 0.2008(3) 0.3998(4) 0.40679(9) 0.0292(10) Uani 1 1 d . . . . .
H20A H 0.1597 0.4310 0.4021 0.044 Uiso 1 1 calc R U . . .
H20B H 0.2401 0.4332 0.4217 0.044 Uiso 1 1 calc R U . . .
H20C H 0.1554 0.3266 0.4100 0.044 Uiso 1 1 calc R U . . .
C21 C 0.3445(4) 0.5278(3) 0.37993(10) 0.0336(11) Uani 1 1 d . . . . .
H21A H 0.3962 0.5362 0.3678 0.050 Uiso 1 1 calc R U . . .
H21B H 0.3785 0.5644 0.3950 0.050 Uiso 1 1 calc R U . . .
H21C H 0.3030 0.5556 0.3733 0.050 Uiso 1 1 calc R U . . .
C22 C 0.4072(3) 0.4149(3) 0.41431(7) 0.0190(8) Uani 1 1 d . . . . .
H22 H 0.4047 0.4688 0.4228 0.023 Uiso 1 1 calc R U . . .
Sb23 Sb 0.3333 0.6667 0.46484(2) 0.01684(12) Uani 1 3 d S T P . .
F24 F 0.21821(19) 0.6309(2) 0.44559(5) 0.0328(6) Uani 1 1 d . . . . .
F25 F 0.44586(19) 0.6981(2) 0.48545(5) 0.0298(6) Uani 1 1 d . . . . .
Sb26 Sb 0.0000 0.0000 0.37582(2) 0.0487(2) Uani 1 3 d S T P . .
F27 F -0.0008(4) 0.1009(3) 0.39546(10) 0.0848(14) Uani 1 1 d . . . . .
F28 F 0.0994(3) 0.1018(3) 0.35571(9) 0.0713(12) Uani 1 1 d . . . . .
C29 C 0.1856(7) 0.1585(8) 0.44397(18) 0.0710(8) Uani 0.8 1 d . U P . .
H29A H 0.2020 0.2025 0.4292 0.085 Uiso 0.8 1 calc R U P . .
H29B H 0.1409 0.0867 0.4387 0.085 Uiso 0.8 1 calc R U P . .
Cl30 Cl 0.29695(16) 0.17110(17) 0.45554(4) 0.0616(5) Uani 0.8 1 d . U P . .
Cl31 Cl 0.1195(2) 0.1901(3) 0.46411(6) 0.1015(8) Uani 0.8 1 d . U P . .


_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 O10 2.025(3) 2_655 ?
Ni1 O10 2.025(3) . ?
Ni1 O10 2.025(3) 3_665 ?
Ni1 N2 2.047(3) 3_665 ?
Ni1 N2 2.047(3) 2_655 ?
Ni1 N2 2.047(3) . ?
N2 C7 1.344(5) . ?
N2 N3 1.359(4) . ?
N3 C4 1.344(5) . ?
N3 H3 0.8800 . ?
C4 C6 1.365(6) . ?
C4 C5 1.496(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.407(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.461(5) . ?
C8 C22 1.376(5) . ?
C8 C9 1.461(5) . ?
C9 O10 1.258(5) . ?
C9 C11 1.469(5) . ?
C11 C16 1.368(6) . ?
C11 C12 1.533(5) . ?
C12 C14 1.537(6) . ?
C12 C13 1.537(6) . ?
C12 C15 1.546(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.410(6) . ?
C16 H16 0.9500 . ?
C17 C22 1.407(6) . ?
C17 C18 1.523(5) . ?
C18 C19 1.530(6) . ?
C18 C21 1.538(6) . ?
C18 C20 1.547(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 0.9500 . ?
Sb23 F24 1.861(2) . ?
Sb23 F24 1.861(2) 3_565 ?
Sb23 F24 1.861(2) 2_665 ?
Sb23 F25 1.885(2) 2_665 ?
Sb23 F25 1.885(2) 3_565 ?
Sb23 F25 1.885(2) . ?
Sb26 F27 1.864(4) 3 ?
Sb26 F27 1.864(4) . ?
Sb26 F27 1.864(4) 2 ?
Sb26 F28 1.871(4) 2 ?
Sb26 F28 1.871(4) 3 ?
Sb26 F28 1.871(4) . ?
C29 Cl31 1.701(10) . ?
C29 Cl30 1.713(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?

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
O10 Ni1 O10 88.14(11) 2_655 . ?
O10 Ni1 O10 88.14(11) 2_655 3_665 ?
O10 Ni1 O10 88.14(11) . 3_665 ?
O10 Ni1 N2 84.92(12) 2_655 3_665 ?
O10 Ni1 N2 170.73(12) . 3_665 ?
O10 Ni1 N2 85.49(11) 3_665 3_665 ?
O10 Ni1 N2 85.49(11) 2_655 2_655 ?
O10 Ni1 N2 84.92(12) . 2_655 ?
O10 Ni1 N2 170.73(12) 3_665 2_655 ?
N2 Ni1 N2 100.63(11) 3_665 2_655 ?
O10 Ni1 N2 170.73(12) 2_655 . ?
O10 Ni1 N2 85.49(11) . . ?
O10 Ni1 N2 84.92(12) 3_665 . ?
N2 Ni1 N2 100.63(11) 3_665 . ?
N2 Ni1 N2 100.63(11) 2_655 . ?
C7 N2 N3 105.3(3) . . ?
C7 N2 Ni1 126.1(3) . . ?
N3 N2 Ni1 123.3(2) . . ?
C4 N3 N2 112.3(3) . . ?
C4 N3 H3 123.8 . . ?
N2 N3 H3 123.8 . . ?
N3 C4 C6 106.3(4) . . ?
N3 C4 C5 121.8(4) . . ?
C6 C4 C5 131.9(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 C7 106.8(4) . . ?
C4 C6 H6 126.6 . . ?
C7 C6 H6 126.6 . . ?
N2 C7 C6 109.2(3) . . ?
N2 C7 C8 124.0(3) . . ?
C6 C7 C8 126.8(4) . . ?
C22 C8 C9 118.2(3) . . ?
C22 C8 C7 119.1(4) . . ?
C9 C8 C7 122.7(3) . . ?
O10 C9 C8 121.7(3) . . ?
O10 C9 C11 119.3(3) . . ?
C8 C9 C11 119.0(3) . . ?
C9 O10 Ni1 133.8(3) . . ?
C16 C11 C9 118.2(3) . . ?
C16 C11 C12 122.4(3) . . ?
C9 C11 C12 119.3(3) . . ?
C11 C12 C14 109.3(3) . . ?
C11 C12 C13 111.7(3) . . ?
C14 C12 C13 107.6(3) . . ?
C11 C12 C15 110.7(3) . . ?
C14 C12 C15 110.3(3) . . ?
C13 C12 C15 107.2(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 C17 123.1(4) . . ?
C11 C16 H16 118.5 . . ?
C17 C16 H16 118.5 . . ?
C22 C17 C16 118.4(4) . . ?
C22 C17 C18 118.6(4) . . ?
C16 C17 C18 123.0(4) . . ?
C17 C18 C19 113.0(3) . . ?
C17 C18 C21 108.3(3) . . ?
C19 C18 C21 108.3(4) . . ?
C17 C18 C20 108.6(4) . . ?
C19 C18 C20 108.7(4) . . ?
C21 C18 C20 109.9(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C8 C22 C17 122.9(4) . . ?
C8 C22 H22 118.5 . . ?
C17 C22 H22 118.5 . . ?
F24 Sb23 F24 91.45(12) . 3_565 ?
F24 Sb23 F24 91.45(12) . 2_665 ?
F24 Sb23 F24 91.45(12) 3_565 2_665 ?
F24 Sb23 F25 91.25(12) . 2_665 ?
F24 Sb23 F25 89.02(11) 3_565 2_665 ?
F24 Sb23 F25 177.24(12) 2_665 2_665 ?
F24 Sb23 F25 89.02(11) . 3_565 ?
F24 Sb23 F25 177.24(12) 3_565 3_565 ?
F24 Sb23 F25 91.25(12) 2_665 3_565 ?
F25 Sb23 F25 88.25(12) 2_665 3_565 ?
F24 Sb23 F25 177.24(12) . . ?
F24 Sb23 F25 91.25(13) 3_565 . ?
F24 Sb23 F25 89.02(11) 2_665 . ?
F25 Sb23 F25 88.25(12) 2_665 . ?
F25 Sb23 F25 88.25(12) 3_565 . ?
F27 Sb26 F27 90.4(2) 3 . ?
F27 Sb26 F27 90.4(2) 3 2 ?
F27 Sb26 F27 90.4(2) . 2 ?
F27 Sb26 F28 178.9(2) 3 2 ?
F27 Sb26 F28 90.6(2) . 2 ?
F27 Sb26 F28 89.71(19) 2 2 ?
F27 Sb26 F28 89.71(19) 3 3 ?
F27 Sb26 F28 178.9(2) . 3 ?
F27 Sb26 F28 90.6(2) 2 3 ?
F28 Sb26 F28 89.2(2) 2 3 ?
F27 Sb26 F28 90.6(2) 3 . ?
F27 Sb26 F28 89.71(19) . . ?
F27 Sb26 F28 178.9(2) 2 . ?
F28 Sb26 F28 89.2(2) 2 . ?
F28 Sb26 F28 89.2(2) 3 . ?
Cl31 C29 Cl30 114.3(6) . . ?
Cl31 C29 H29A 108.7 . . ?
Cl30 C29 H29A 108.7 . . ?
Cl31 C29 H29B 108.7 . . ?
Cl30 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?

_refine_diff_density_max         1.241
_refine_diff_density_min         -1.631
_refine_diff_density_rms         0.104

_shelxl_version_number           2013-4

