Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2003

data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Pradip K. Mascharak'
'Todd C. Harrop'
'Marilyn M. Olmstead'

_publ_contact_author_name        'Dr Pradip K. Mascharak'
_publ_contact_author_address     
;
Department of Chemistry and Biochemistry
University of CAlifornia
Santa Cruz
California
CA 95064
UNITED STATES OF AMERICA
;

_publ_contact_author_email       ?

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Dioxygen Activation by a Dinuclear Nickel Thiolate
Complex:  Structural Characterization of the Ligand Oxidized Product
;

data_mn1263
_database_code_CSD               198289

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            (Et4N)2[Ni2(ArPSO)2]
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H56 N4 Ni2 O4 S2'
_chemical_formula_weight         862.45

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'
S S 0.1246 0.1234 '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           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'

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

_cell_length_a                   13.0112(10)
_cell_length_b                   13.8925(11)
_cell_length_c                   22.1485(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4003.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    91(2)
_cell_measurement_reflns_used    999
_cell_measurement_theta_min      3.5
_cell_measurement_theta_max      29.8

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7719
_exptl_absorpt_correction_T_max  0.9680
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'

_exptl_special_details           
; 
? 
;

_diffrn_ambient_temperature      91(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 8.3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38325
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_sigmaI/netI    0.052
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         31.50
_reflns_number_total             6376
_reflns_number_gt                4041
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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/[\s^2^(Fo^2^)+(0.0532P)^2^+4.3804P] where P=(Fo^2^+2Fc^2^)/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         6376
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1286
_refine_ls_wR_factor_gt          0.1041
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_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 0.96358(2) 0.16892(2) 0.691657(15) 0.02408(9) Uani 1 1 d . . .
S1 S 0.89632(5) 0.10186(4) 0.77045(3) 0.02842(15) Uani 1 1 d . . .
O1 O 1.03530(14) 0.22411(13) 0.62903(8) 0.0299(4) Uani 1 1 d . . .
O2 O 0.71421(17) 0.2642(2) 0.60496(10) 0.0545(7) Uani 1 1 d . . .
N1 N 0.83701(16) 0.22978(15) 0.67593(10) 0.0267(4) Uani 1 1 d . . .
C1 C 0.9935(2) 0.26916(18) 0.58313(12) 0.0294(5) Uani 1 1 d . . .
C2 C 1.0614(3) 0.3053(2) 0.53859(13) 0.0384(7) Uani 1 1 d . . .
H2 H 1.1334 0.3001 0.5450 0.046 Uiso 1 1 calc R . .
C3 C 1.0265(3) 0.3475(2) 0.48647(15) 0.0489(9) Uani 1 1 d . . .
H3 H 1.0737 0.3710 0.4573 0.059 Uiso 1 1 calc R . .
C4 C 0.9210(4) 0.3554(3) 0.47692(16) 0.0590(10) Uani 1 1 d . . .
H4 H 0.8959 0.3837 0.4407 0.071 Uiso 1 1 calc R . .
C5 C 0.8535(3) 0.3226(3) 0.51960(14) 0.0496(9) Uani 1 1 d . . .
H5 H 0.7819 0.3285 0.5122 0.060 Uiso 1 1 calc R . .
C6 C 0.8863(2) 0.2803(2) 0.57425(12) 0.0330(6) Uani 1 1 d . . .
C7 C 0.8055(2) 0.2559(2) 0.61923(13) 0.0349(6) Uani 1 1 d . . .
C8 C 0.76842(19) 0.23629(19) 0.72532(12) 0.0277(5) Uani 1 1 d . . .
C9 C 0.6839(2) 0.2987(2) 0.72870(13) 0.0339(6) Uani 1 1 d . . .
H9 H 0.6638 0.3344 0.6941 0.041 Uiso 1 1 calc R . .
C10 C 0.6293(2) 0.3087(2) 0.78211(14) 0.0382(7) Uani 1 1 d . . .
H10 H 0.5730 0.3522 0.7837 0.046 Uiso 1 1 calc R . .
C11 C 0.6551(2) 0.2567(2) 0.83305(14) 0.0367(6) Uani 1 1 d . . .
H11 H 0.6168 0.2641 0.8693 0.044 Uiso 1 1 calc R . .
C12 C 0.7376(2) 0.1937(2) 0.83071(13) 0.0330(6) Uani 1 1 d . . .
H12 H 0.7562 0.1574 0.8654 0.040 Uiso 1 1 calc R . .
C13 C 0.79296(19) 0.18379(18) 0.77725(12) 0.0279(5) Uani 1 1 d . . .
N2 N 1.0000 0.0000 0.5000 0.0266(6) Uiso 1 2 d S . .
C14 C 0.9768(4) -0.0904(4) 0.5346(2) 0.0269(10) Uiso 0.50 1 d P A -1
H14A H 1.0304 -0.1390 0.5258 0.032 Uiso 0.50 1 calc PR A -1
H14B H 0.9100 -0.1167 0.5208 0.032 Uiso 0.50 1 calc PR A -1
C15 C 0.9721(6) -0.0733(6) 0.6032(4) 0.0430(18) Uiso 0.50 1 d P A -1
H15A H 0.9565 -0.1341 0.6238 0.065 Uiso 0.50 1 calc PR A -1
H15B H 0.9182 -0.0261 0.6123 0.065 Uiso 0.50 1 calc PR A -1
H15C H 1.0385 -0.0488 0.6173 0.065 Uiso 0.50 1 calc PR A -1
C16 C 1.1079(4) 0.0401(4) 0.5247(2) 0.0272(10) Uiso 0.50 1 d P A -1
H16A H 1.1297 0.0941 0.4985 0.033 Uiso 0.50 1 calc PR A -1
H16B H 1.0969 0.0664 0.5657 0.033 Uiso 0.50 1 calc PR A -1
C17 C 1.1933(6) -0.0306(5) 0.5276(3) 0.0411(16) Uiso 0.50 1 d P A -1
H17A H 1.2553 0.0011 0.5430 0.062 Uiso 0.50 1 calc PR A -1
H17B H 1.2069 -0.0560 0.4871 0.062 Uiso 0.50 1 calc PR A -1
H17C H 1.1742 -0.0836 0.5545 0.062 Uiso 0.50 1 calc PR A -1
C18 C 0.9292(5) 0.0793(4) 0.5080(3) 0.0357(12) Uiso 0.50 1 d P A -1
H18A H 0.9534 0.1349 0.4840 0.043 Uiso 0.50 1 calc PR A -1
H18B H 0.9291 0.0986 0.5510 0.043 Uiso 0.50 1 calc PR A -1
C19 C 0.8185(7) 0.0543(7) 0.4889(4) 0.062(2) Uiso 0.50 1 d P A -1
H19A H 0.7741 0.1105 0.4949 0.094 Uiso 0.50 1 calc PR A -1
H19B H 0.7931 0.0005 0.5134 0.094 Uiso 0.50 1 calc PR A -1
H19C H 0.8177 0.0359 0.4461 0.094 Uiso 0.50 1 calc PR A -1
C20 C 1.0201(4) -0.0286(4) 0.4347(3) 0.0334(12) Uiso 0.50 1 d P A -1
H20A H 0.9559 -0.0542 0.4169 0.040 Uiso 0.50 1 calc PR A -1
H20B H 1.0721 -0.0806 0.4338 0.040 Uiso 0.50 1 calc PR A -1
C21 C 1.0585(7) 0.0565(6) 0.3958(4) 0.050(2) Uiso 0.50 1 d P A -1
H21A H 1.0711 0.0343 0.3545 0.075 Uiso 0.50 1 calc PR A -1
H21B H 1.1224 0.0819 0.4130 0.075 Uiso 0.50 1 calc PR A -1
H21C H 1.0062 0.1074 0.3953 0.075 Uiso 0.50 1 calc PR A -1
N3 N 1.0000 0.4850(2) 0.7500 0.0226(6) Uani 1 2 d S . .
C22 C 1.0670(2) 0.55100(17) 0.78806(12) 0.0261(5) Uani 1 1 d . . .
H22A H 1.1069 0.5928 0.7605 0.031 Uiso 1 1 calc R . .
H22B H 1.0214 0.5933 0.8121 0.031 Uiso 1 1 calc R . .
C23 C 1.1411(2) 0.5026(2) 0.83063(13) 0.0374(6) Uani 1 1 d . . .
H23A H 1.1028 0.4617 0.8589 0.056 Uiso 1 1 calc R . .
H23B H 1.1793 0.5515 0.8532 0.056 Uiso 1 1 calc R . .
H23C H 1.1893 0.4628 0.8075 0.056 Uiso 1 1 calc R . .
C24 C 0.9358(2) 0.41743(18) 0.78885(12) 0.0278(5) Uani 1 1 d . . .
H24A H 0.8973 0.3737 0.7617 0.033 Uiso 1 1 calc R . .
H24B H 0.9832 0.3772 0.8131 0.033 Uiso 1 1 calc R . .
C25 C 0.8605(2) 0.4640(2) 0.83106(14) 0.0364(6) Uani 1 1 d . . .
H25A H 0.8973 0.5066 0.8590 0.055 Uiso 1 1 calc R . .
H25B H 0.8242 0.4142 0.8541 0.055 Uiso 1 1 calc R . .
H25C H 0.8107 0.5017 0.8077 0.055 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.02251(15) 0.02145(15) 0.02828(17) -0.00299(13) 0.00008(13) -0.00089(13)
S1 0.0263(3) 0.0223(3) 0.0367(3) 0.0006(3) 0.0018(3) -0.0031(2)
O1 0.0287(9) 0.0320(10) 0.0291(9) 0.0006(8) 0.0001(8) -0.0001(8)
O2 0.0349(12) 0.0916(19) 0.0372(12) -0.0228(13) -0.0155(9) 0.0151(12)
N1 0.0236(11) 0.0255(10) 0.0311(11) -0.0053(9) -0.0018(8) -0.0019(8)
C1 0.0400(15) 0.0230(11) 0.0251(13) -0.0075(10) -0.0016(11) 0.0006(11)
C2 0.0513(19) 0.0301(14) 0.0337(15) -0.0015(11) 0.0012(13) -0.0053(13)
C3 0.073(3) 0.0415(18) 0.0320(16) 0.0044(13) 0.0020(16) -0.0045(17)
C4 0.089(3) 0.057(2) 0.0302(17) 0.0093(15) -0.0063(18) 0.011(2)
C5 0.060(2) 0.056(2) 0.0330(16) -0.0043(15) -0.0144(15) 0.0175(17)
C6 0.0434(16) 0.0318(14) 0.0239(12) -0.0085(11) -0.0061(11) 0.0068(12)
C7 0.0330(14) 0.0403(15) 0.0313(14) -0.0142(12) -0.0103(11) 0.0046(12)
C8 0.0199(12) 0.0285(12) 0.0348(14) -0.0063(11) -0.0023(10) -0.0051(10)
C9 0.0241(13) 0.0409(15) 0.0367(15) -0.0038(12) -0.0054(11) -0.0001(11)
C10 0.0223(13) 0.0449(17) 0.0472(17) -0.0056(14) 0.0002(12) 0.0038(12)
C11 0.0260(14) 0.0438(16) 0.0402(16) -0.0084(13) 0.0064(11) -0.0045(12)
C12 0.0269(13) 0.0354(14) 0.0368(14) -0.0016(12) -0.0005(11) -0.0084(11)
C13 0.0210(11) 0.0275(13) 0.0352(14) -0.0027(10) -0.0013(10) -0.0066(10)
N3 0.0262(14) 0.0174(13) 0.0242(14) 0.000 -0.0011(11) 0.000
C22 0.0309(13) 0.0209(11) 0.0264(12) -0.0040(9) -0.0004(10) -0.0031(10)
C23 0.0396(16) 0.0391(16) 0.0337(14) -0.0028(12) -0.0102(13) 0.0012(13)
C24 0.0329(13) 0.0232(12) 0.0274(12) 0.0060(10) -0.0012(10) -0.0058(10)
C25 0.0371(16) 0.0364(15) 0.0357(15) 0.0046(12) 0.0076(12) -0.0005(12)

_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 1.8393(19) . ?
Ni1 N1 1.884(2) . ?
Ni1 S1 2.1632(7) . ?
Ni1 S1 2.2124(7) 3_756 ?
Ni1 Ni1 2.7527(7) 3_756 ?
S1 C13 1.768(3) . ?
S1 Ni1 2.2124(7) 3_756 ?
O1 C1 1.312(3) . ?
O2 C7 1.235(3) . ?
N1 C7 1.370(4) . ?
N1 C8 1.415(3) . ?
C1 C2 1.416(4) . ?
C1 C6 1.417(4) . ?
C2 C3 1.372(4) . ?
C3 C4 1.394(6) . ?
C4 C5 1.368(5) . ?
C5 C6 1.412(4) . ?
C6 C7 1.487(4) . ?
C8 C13 1.399(4) . ?
C8 C9 1.403(4) . ?
C9 C10 1.387(4) . ?
C10 C11 1.381(4) . ?
C11 C12 1.386(4) . ?
C12 C13 1.393(4) . ?
N2 C18 1.447(6) . ?
N2 C18 1.447(6) 5_756 ?
N2 C14 1.502(5) 5_756 ?
N2 C14 1.502(5) . ?
N2 C20 1.523(6) . ?
N2 C20 1.523(6) 5_756 ?
N2 C16 1.606(5) 5_756 ?
N2 C16 1.606(5) . ?
C14 C15 1.540(9) . ?
C16 C17 1.485(9) . ?
C18 C19 1.541(11) . ?
C20 C21 1.546(10) . ?
N3 C22 1.521(3) 3_756 ?
N3 C22 1.521(3) . ?
N3 C24 1.523(3) 3_756 ?
N3 C24 1.523(3) . ?
C22 C23 1.507(4) . ?
C24 C25 1.501(4) . ?

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 N1 96.71(9) . . ?
O1 Ni1 S1 173.34(6) . . ?
N1 Ni1 S1 89.36(7) . . ?
O1 Ni1 S1 92.50(6) . 3_756 ?
N1 Ni1 S1 168.37(7) . 3_756 ?
S1 Ni1 S1 81.14(3) . 3_756 ?
O1 Ni1 Ni1 122.24(6) . 3_756 ?
N1 Ni1 Ni1 118.34(7) . 3_756 ?
S1 Ni1 Ni1 51.82(2) . 3_756 ?
S1 Ni1 Ni1 50.22(2) 3_756 3_756 ?
C13 S1 Ni1 95.69(9) . . ?
C13 S1 Ni1 108.86(9) . 3_756 ?
Ni1 S1 Ni1 77.96(3) . 3_756 ?
C1 O1 Ni1 124.96(18) . . ?
C7 N1 C8 120.2(2) . . ?
C7 N1 Ni1 123.35(19) . . ?
C8 N1 Ni1 115.92(17) . . ?
O1 C1 C2 116.7(3) . . ?
O1 C1 C6 124.6(3) . . ?
C2 C1 C6 118.6(3) . . ?
C3 C2 C1 122.1(3) . . ?
C2 C3 C4 119.2(3) . . ?
C5 C4 C3 120.1(3) . . ?
C4 C5 C6 122.5(3) . . ?
C5 C6 C1 117.5(3) . . ?
C5 C6 C7 117.1(3) . . ?
C1 C6 C7 125.3(2) . . ?
O2 C7 N1 123.2(3) . . ?
O2 C7 C6 119.1(3) . . ?
N1 C7 C6 117.6(2) . . ?
C13 C8 C9 117.2(2) . . ?
C13 C8 N1 117.3(2) . . ?
C9 C8 N1 125.1(3) . . ?
C10 C9 C8 120.6(3) . . ?
C11 C10 C9 121.3(3) . . ?
C10 C11 C12 119.2(3) . . ?
C11 C12 C13 119.6(3) . . ?
C12 C13 C8 122.0(3) . . ?
C12 C13 S1 122.0(2) . . ?
C8 C13 S1 116.1(2) . . ?
C18 N2 C18 180.000(1) . 5_756 ?
C18 N2 C14 63.5(3) . 5_756 ?
C18 N2 C14 116.5(3) 5_756 5_756 ?
C18 N2 C14 116.5(3) . . ?
C18 N2 C14 63.5(3) 5_756 . ?
C14 N2 C14 180.000(1) 5_756 . ?
C18 N2 C20 115.1(3) . . ?
C18 N2 C20 64.9(3) 5_756 . ?
C14 N2 C20 72.5(3) 5_756 . ?
C14 N2 C20 107.5(3) . . ?
C18 N2 C20 64.9(3) . 5_756 ?
C18 N2 C20 115.1(3) 5_756 5_756 ?
C14 N2 C20 107.5(3) 5_756 5_756 ?
C14 N2 C20 72.5(3) . 5_756 ?
C20 N2 C20 180.00(13) . 5_756 ?
C18 N2 C16 75.4(3) . 5_756 ?
C18 N2 C16 104.6(3) 5_756 5_756 ?
C14 N2 C16 107.0(3) 5_756 5_756 ?
C14 N2 C16 73.0(3) . 5_756 ?
C20 N2 C16 74.7(3) . 5_756 ?
C20 N2 C16 105.3(3) 5_756 5_756 ?
C18 N2 C16 104.6(3) . . ?
C18 N2 C16 75.4(3) 5_756 . ?
C14 N2 C16 73.0(3) 5_756 . ?
C14 N2 C16 107.0(3) . . ?
C20 N2 C16 105.3(3) . . ?
C20 N2 C16 74.7(3) 5_756 . ?
C16 N2 C16 180.0(4) 5_756 . ?
N2 C14 C15 112.5(4) . . ?
C17 C16 N2 116.1(4) . . ?
N2 C18 C19 113.0(5) . . ?
N2 C20 C21 112.7(5) . . ?
C22 N3 C22 105.8(3) 3_756 . ?
C22 N3 C24 111.89(14) 3_756 3_756 ?
C22 N3 C24 111.76(14) . 3_756 ?
C22 N3 C24 111.76(14) 3_756 . ?
C22 N3 C24 111.89(14) . . ?
C24 N3 C24 103.9(3) 3_756 . ?
C23 C22 N3 116.4(2) . . ?
C25 C24 N3 116.4(2) . . ?

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        31.50
_diffrn_measured_fraction_theta_full 0.958
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.090