Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2002

data_global

_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'Bencini, Andrea'
'Bazzicalupi, Carla'
'Bellusci, Annalisa'
'Berni, Emanuela'
'Bianchi, Antonio' 
'Ciattini, Samuele'
'Giorgi, Claudia'
'Valtancoli, Barbara'

_publ_contact_author_name     	'Dr Andrea Bencini'  
_publ_contact_author_address 
;
Dept of Chemistry
University of Florence
Via della Lastruccia 3
Sesto Fiorentino
Firenze
50019
ITALY
;

_publ_contact_author_email       'ANDREA.BENCINI@UNIFI.IT'

_publ_section_title		
;
A New Dipyridine-containing Cryptand for both Proton and Cu(II)
Encapsulation. A Solution and Solid State Study
;

data_[CuLH](ClO4)3.2H2O
_database_code_CSD                  177616

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety
;
(C24 H37 N6 Cu 3+), (Cl O4 1-)3, (H2 O)2
;
_chemical_formula_sum
'C24 H41 Cl3 Cu N6 O14'
_chemical_formula_weight          807.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C'  'C'   0.0181   0.0091
'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'   0.0311   0.0180
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O'  'O'   0.0492   0.0322
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl'  'Cl'   0.3639   0.7018
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cu'  'Cu'  -1.9646   0.5888
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    C2/c

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

_cell_length_a                    29.500(7)
_cell_length_b                    17.825(7)
_cell_length_c                    13.781(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  104.193(10)
_cell_angle_gamma                 90.00
_cell_volume                      7025(4)
_cell_formula_units_Z             8
_cell_measurement_temperature     298
_cell_measurement_reflns_used     21
_cell_measurement_theta_min       15
_cell_measurement_theta_max       45

_exptl_crystal_description        prismatic
_exptl_crystal_colour             blue
_exptl_crystal_size_max           0.4
_exptl_crystal_size_mid           0.3
_exptl_crystal_size_min           0.2
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.527
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              3352
_exptl_absorpt_coefficient_mu     3.606
_exptl_absorpt_correction_type    'empirical'
_exptl_absorpt_correction_T_min   0.27
_exptl_absorpt_correction_T_max   0.47
_exptl_absorpt_process_details    'PSI-scan'

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       298
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_radiation_source          'rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'SIEMENS P4'
_diffrn_measurement_method        '\q/2\q'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          3
_diffrn_standards_interval_count  200
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0
_diffrn_reflns_number             11338
_diffrn_reflns_av_R_equivalents   0.0105
_diffrn_reflns_av_sigmaI/netI     0.0237
_diffrn_reflns_limit_h_min        -33
_diffrn_reflns_limit_h_max        1
_diffrn_reflns_limit_k_min        -1
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          2.92
_diffrn_reflns_theta_max          60.83
_reflns_number_total              4936
_reflns_number_gt                 4390
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'XSCANS-Bruker'
_computing_cell_refinement        'XSCANS-Bruker'
_computing_data_reduction         'XSCANS-Bruker'
_computing_structure_solution     'SIR97 (Altomare, 1999)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 (Ver. 1.01\b) (Farrugia, 1997)'
_computing_publication_material   'Parst97 (Nardelli, 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.

Two perchlorate anions (Cl1 and Cl2) are located in special position on
crystallographic axis (symmetry opertaion: -x+1, y, -z+0.5 for Cl1 and
-x+1, y, -z+1.5 for Cl2). In particular, the Cl1 perchlorate is disordered,
with the crystallographic axis passing along the Cl1-O11 bond, and the
crystallographic symmetry is simulated by two different tetrahedrons
which have in common the Cl1-O1 bond.
;

_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^)+(0.1328P)^2^+49.7003P] 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
_atom_sites_solution_H100         geom
_refine_ls_H100_treatment         refall
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          4936
_refine_ls_number_parameters      463
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0855
_refine_ls_R_factor_gt            0.0782
_refine_ls_wR_factor_ref          0.2302
_refine_ls_wR_factor_gt           0.2193
_refine_ls_goodness_of_fit_ref    1.012
_refine_ls_restrained_S_all       1.012
_refine_ls_shift/su_max           0.009
_refine_ls_shift/su_mean          0.001

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 0.40499(3) 0.24265(4) 0.49903(6) 0.0422(3) Uani 1 1 d . . .
N1 N 0.46794(17) 0.2093(3) 0.5026(3) 0.0490(12) Uani 1 1 d . . .
N2 N 0.43894(15) 0.3336(3) 0.5478(3) 0.0450(11) Uani 1 1 d . . .
C1 C 0.4860(2) 0.3316(4) 0.5628(4) 0.0545(15) Uani 1 1 d . . .
C2 C 0.5033(2) 0.2585(4) 0.5359(4) 0.0509(15) Uani 1 1 d . . .
C3 C 0.4750(2) 0.1413(4) 0.4702(4) 0.0554(15) Uani 1 1 d . . .
C4 C 0.5198(3) 0.1172(5) 0.4711(5) 0.070(2) Uani 1 1 d . . .
H4 H 0.5249 0.0697 0.4480 0.084 Uiso 1 1 calc R . .
C5 C 0.5563(3) 0.1648(5) 0.5068(5) 0.075(2) Uani 1 1 d . . .
H5 H 0.5866 0.1489 0.5097 0.090 Uiso 1 1 calc R . .
C6 C 0.5490(2) 0.2367(5) 0.5389(5) 0.068(2) Uani 1 1 d . . .
H6 H 0.5739 0.2694 0.5618 0.082 Uiso 1 1 calc R . .
C7 C 0.5122(3) 0.3949(5) 0.5963(5) 0.074(2) Uani 1 1 d . . .
H7 H 0.5446 0.3949 0.6066 0.089 Uiso 1 1 calc R . .
C8 C 0.4883(3) 0.4583(5) 0.6137(6) 0.085(2) Uani 1 1 d . . .
H8 H 0.5052 0.5011 0.6386 0.103 Uiso 1 1 calc R . .
C9 C 0.4402(3) 0.4598(4) 0.5954(5) 0.0683(18) Uani 1 1 d . . .
H9 H 0.4244 0.5031 0.6059 0.082 Uiso 1 1 calc R . .
C10 C 0.4162(2) 0.3947(3) 0.5608(4) 0.0518(14) Uani 1 1 d . . .
C11 C 0.3641(2) 0.3857(4) 0.5395(5) 0.0564(15) Uani 1 1 d . . .
H11A H 0.3492 0.4295 0.5035 0.068 Uiso 1 1 calc R . .
H11B H 0.3549 0.3828 0.6023 0.068 Uiso 1 1 calc R . .
N3 N 0.34763(16) 0.3165(3) 0.4787(3) 0.0480(11) Uani 1 1 d . . .
C12 C 0.3119(2) 0.2763(4) 0.5178(5) 0.0600(16) Uani 1 1 d . . .
H12A H 0.2964 0.2398 0.4686 0.072 Uiso 1 1 calc R . .
H12B H 0.2885 0.3120 0.5275 0.072 Uiso 1 1 calc R . .
C13 C 0.3326(3) 0.2365(5) 0.6161(5) 0.072(2) Uani 1 1 d . . .
H13A H 0.3400 0.2734 0.6694 0.087 Uiso 1 1 calc R . .
H13B H 0.3093 0.2027 0.6307 0.087 Uiso 1 1 calc R . .
N4 N 0.37535(19) 0.1933(3) 0.6148(4) 0.0581(13) Uani 1 1 d . . .
C14 C 0.3666(3) 0.1135(4) 0.5842(5) 0.073(2) Uani 1 1 d . . .
H14A H 0.3420 0.0937 0.6124 0.088 Uiso 1 1 calc R . .
H14B H 0.3947 0.0844 0.6107 0.088 Uiso 1 1 calc R . .
C15 C 0.3524(3) 0.1055(4) 0.4713(5) 0.0671(18) Uani 1 1 d . . .
H15A H 0.3497 0.0527 0.4540 0.081 Uiso 1 1 calc R . .
H15B H 0.3220 0.1285 0.4459 0.081 Uiso 1 1 calc R . .
N5 N 0.38719(17) 0.1417(3) 0.4227(4) 0.0505(12) Uani 1 1 d . . .
C16 C 0.4312(2) 0.0944(4) 0.4399(5) 0.0642(17) Uani 1 1 d . . .
H16A H 0.4310 0.0578 0.4920 0.077 Uiso 1 1 calc R . .
H16B H 0.4315 0.0673 0.3790 0.077 Uiso 1 1 calc R . .
C17 C 0.4077(3) 0.1962(5) 0.7153(5) 0.082(2) Uani 1 1 d . . .
H17A H 0.4112 0.2473 0.7382 0.123 Uiso 1 1 calc R . .
H17B H 0.4377 0.1768 0.7120 0.123 Uiso 1 1 calc R . .
H17C H 0.3954 0.1665 0.7610 0.123 Uiso 1 1 calc R . .
C18 C 0.3281(2) 0.3368(4) 0.3716(4) 0.0522(14) Uani 1 1 d . . .
H18A H 0.3060 0.3775 0.3677 0.063 Uiso 1 1 calc R . .
H18B H 0.3114 0.2940 0.3365 0.063 Uiso 1 1 calc R . .
C19 C 0.3658(2) 0.3604(3) 0.3202(4) 0.0517(14) Uani 1 1 d . . .
H19A H 0.3760 0.4108 0.3418 0.062 Uiso 1 1 calc R . .
H19B H 0.3925 0.3273 0.3418 0.062 Uiso 1 1 calc R . .
C20 C 0.3506(2) 0.3591(4) 0.2073(5) 0.0587(16) Uani 1 1 d . . .
H20A H 0.3246 0.3935 0.1864 0.070 Uiso 1 1 calc R . .
H20B H 0.3761 0.3784 0.1815 0.070 Uiso 1 1 calc R . .
N6 N 0.3363(2) 0.2850(4) 0.1590(4) 0.0585(15) Uani 1 1 d . . .
C21 C 0.3739(3) 0.2273(4) 0.1608(5) 0.0679(18) Uani 1 1 d . . .
H21A H 0.3976 0.2500 0.1325 0.081 Uiso 1 1 calc R . .
H21B H 0.3601 0.1864 0.1169 0.081 Uiso 1 1 calc R . .
C22 C 0.3980(2) 0.1940(4) 0.2613(5) 0.0611(16) Uani 1 1 d . . .
H22A H 0.4128 0.2343 0.3050 0.073 Uiso 1 1 calc R . .
H22B H 0.4226 0.1607 0.2518 0.073 Uiso 1 1 calc R . .
C23 C 0.3666(2) 0.1508(4) 0.3135(4) 0.0579(16) Uani 1 1 d . . .
H23A H 0.3369 0.1768 0.3036 0.070 Uiso 1 1 calc R . .
H23B H 0.3605 0.1015 0.2831 0.070 Uiso 1 1 calc R . .
C24 C 0.3117(3) 0.2979(6) 0.0502(5) 0.089(3) Uani 1 1 d . . .
H24A H 0.2877 0.3350 0.0459 0.133 Uiso 1 1 calc R . .
H24B H 0.2979 0.2518 0.0212 0.133 Uiso 1 1 calc R . .
H24C H 0.3339 0.3151 0.0146 0.133 Uiso 1 1 calc R . .
Cl1 Cl 0.5000 0.33731(12) 0.2500 0.0613(6) Uani 1 2 d S . .
O11 O 0.5000 0.2591(5) 0.2500 0.142(5) Uani 1 2 d S . .
O12 O 0.4618(4) 0.3801(8) 0.2493(18) 0.109(5) Uani 0.50 1 d P . .
O13 O 0.4780(6) 0.3546(9) 0.3267(11) 0.107(5) Uani 0.50 1 d P . .
O14 O 0.4625(6) 0.3567(9) 0.1557(11) 0.119(5) Uani 0.50 1 d P . .
Cl2 Cl 0.5000 0.01759(14) 0.7500 0.0676(7) Uani 1 2 d S . .
O21 O 0.5004(3) 0.0589(5) 0.8349(4) 0.123(3) Uani 1 1 d . . .
O22 O 0.5403(4) -0.0265(6) 0.7713(6) 0.167(4) Uani 1 1 d . . .
Cl3 Cl 0.34639(7) 0.41829(10) 0.82956(15) 0.0738(5) Uani 1 1 d . . .
O31 O 0.3502(4) 0.3430(4) 0.8349(7) 0.149(3) Uani 1 1 d . . .
O32 O 0.3731(4) 0.4500(5) 0.7709(7) 0.175(4) Uani 1 1 d . . .
O33 O 0.3573(8) 0.4482(8) 0.9185(10) 0.305(11) Uani 1 1 d . . .
O34 O 0.3055(6) 0.4323(15) 0.793(2) 0.419(17) Uani 1 1 d . . .
Cl4 Cl 0.30601(7) -0.10210(11) 0.36185(17) 0.0835(6) Uani 1 1 d . . .
O41 O 0.3204(4) -0.1776(5) 0.3563(11) 0.207(6) Uani 1 1 d . . .
O42 O 0.3362(4) -0.0573(5) 0.3250(9) 0.180(4) Uani 1 1 d . . .
O43 O 0.3159(7) -0.0895(8) 0.4599(10) 0.256(8) Uani 1 1 d . . .
O44 O 0.2634(3) -0.0914(12) 0.3317(17) 0.363(13) Uani 1 1 d . . .
O100 O 0.2577(2) 0.2145(4) 0.2038(5) 0.109(2) Uani 1 1 d . . .
O200 O 0.2445(5) 0.0520(12) 0.487(2) 0.244(16) Uani 0.50 1 d P . .
O300 O 0.2247(8) 0.447(2) 0.851(2) 0.230(12) Uani 0.50 1 d P . .
H100 H 0.3175(17) 0.269(3) 0.175(3) 0.010(13) Uiso 1 1 d . . .

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
Cu1 0.0394(5) 0.0397(5) 0.0461(5) -0.0061(3) 0.0077(4) -0.0012(3)
N1 0.053(3) 0.052(3) 0.041(2) 0.001(2) 0.010(2) 0.000(2)
N2 0.039(2) 0.047(3) 0.048(3) -0.008(2) 0.008(2) -0.005(2)
C1 0.059(4) 0.061(4) 0.042(3) -0.005(3) 0.008(3) -0.015(3)
C2 0.041(3) 0.071(4) 0.040(3) 0.007(3) 0.008(2) 0.004(3)
C3 0.067(4) 0.057(4) 0.039(3) 0.004(3) 0.006(3) 0.017(3)
C4 0.078(5) 0.081(5) 0.055(4) 0.014(3) 0.022(4) 0.046(4)
C5 0.054(4) 0.112(7) 0.060(4) 0.016(4) 0.016(3) 0.032(4)
C6 0.044(4) 0.109(6) 0.048(4) 0.018(4) 0.005(3) -0.001(4)
C7 0.067(4) 0.083(5) 0.068(4) -0.009(4) 0.009(4) -0.027(4)
C8 0.106(7) 0.070(5) 0.081(5) -0.021(4) 0.024(5) -0.039(5)
C9 0.082(5) 0.049(4) 0.076(4) -0.018(3) 0.025(4) -0.012(3)
C10 0.064(4) 0.045(4) 0.046(3) -0.009(3) 0.014(3) -0.004(3)
C11 0.056(4) 0.052(4) 0.063(4) -0.013(3) 0.017(3) 0.009(3)
N3 0.047(3) 0.052(3) 0.046(2) -0.002(2) 0.014(2) -0.001(2)
C12 0.049(3) 0.069(4) 0.068(4) 0.001(3) 0.027(3) 0.005(3)
C13 0.077(5) 0.087(5) 0.061(4) 0.004(4) 0.033(4) -0.003(4)
N4 0.071(3) 0.058(3) 0.046(3) 0.001(2) 0.015(2) -0.004(3)
C14 0.101(6) 0.055(4) 0.069(4) 0.008(3) 0.031(4) -0.013(4)
C15 0.088(5) 0.047(4) 0.067(4) -0.002(3) 0.020(4) -0.019(3)
N5 0.060(3) 0.040(3) 0.050(3) 0.000(2) 0.011(2) -0.004(2)
C16 0.081(5) 0.049(4) 0.062(4) -0.007(3) 0.015(3) 0.020(3)
C17 0.101(6) 0.091(6) 0.048(4) 0.003(4) 0.007(4) -0.001(5)
C18 0.045(3) 0.061(4) 0.051(3) 0.004(3) 0.011(3) 0.004(3)
C19 0.051(3) 0.047(3) 0.058(3) -0.001(3) 0.016(3) -0.002(3)
C20 0.059(4) 0.055(4) 0.061(4) 0.012(3) 0.013(3) 0.003(3)
N6 0.054(3) 0.076(4) 0.047(3) 0.007(3) 0.016(3) -0.008(3)
C21 0.072(4) 0.075(5) 0.061(4) -0.007(3) 0.024(3) 0.008(4)
C22 0.061(4) 0.063(4) 0.061(4) -0.005(3) 0.018(3) 0.007(3)
C23 0.065(4) 0.053(4) 0.051(3) -0.007(3) 0.006(3) -0.002(3)
C24 0.086(5) 0.131(8) 0.042(4) 0.008(4) 0.004(3) 0.003(5)
Cl1 0.0616(13) 0.0501(13) 0.0772(15) 0.000 0.0268(11) 0.000
O11 0.101(7) 0.066(6) 0.263(16) 0.000 0.054(9) 0.000
O12 0.045(6) 0.096(9) 0.194(18) -0.003(11) 0.046(9) 0.019(6)
O13 0.137(13) 0.112(11) 0.087(9) -0.025(8) 0.058(9) -0.019(9)
O14 0.121(12) 0.126(11) 0.091(9) 0.023(8) -0.007(8) -0.010(9)
Cl2 0.0881(17) 0.0725(15) 0.0429(11) 0.000 0.0172(10) 0.000
O21 0.148(6) 0.146(6) 0.070(4) -0.039(4) 0.017(4) 0.029(5)
O22 0.192(8) 0.192(9) 0.127(6) 0.032(6) 0.062(6) 0.120(7)
Cl3 0.0780(12) 0.0539(10) 0.0911(13) -0.0059(9) 0.0238(10) 0.0038(8)
O31 0.216(9) 0.070(4) 0.169(8) -0.015(4) 0.063(7) 0.008(5)
O32 0.255(12) 0.151(8) 0.161(8) -0.020(6) 0.132(8) -0.078(8)
O33 0.62(3) 0.185(11) 0.177(11) -0.110(9) 0.228(16) -0.184(17)
O34 0.172(14) 0.40(3) 0.63(5) 0.20(3) 0.01(2) 0.119(17)
Cl4 0.0853(13) 0.0693(13) 0.0985(14) -0.0158(10) 0.0278(11) -0.0071(10)
O41 0.221(11) 0.091(6) 0.354(17) -0.031(8) 0.156(12) -0.024(6)
O42 0.245(12) 0.120(7) 0.222(11) -0.027(7) 0.148(10) -0.051(7)
O43 0.45(3) 0.184(11) 0.157(10) -0.033(9) 0.125(13) -0.046(14)
O44 0.066(6) 0.44(3) 0.52(3) 0.20(2) -0.062(10) 0.024(10)
O100 0.073(4) 0.116(5) 0.123(5) 0.024(4) -0.002(3) -0.025(3)
O200 0.085(10) 0.137(15) 0.52(5) -0.12(2) 0.097(18) 0.015(10)
O300 0.135(16) 0.32(3) 0.22(2) -0.07(2) 0.007(15) 0.004(19)

_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.

Weighted least-squares planes through the starred atoms
(Nardelli, Musatti, Domiano & Andreetti Ric.Sci.(1965),15(II-A),807).
Equation of the plane: m1*X+m2*Y+m3*Z=d

Plane  1
m1 =    .27666( .00162)
m2 =    .34909( .00156)
m3 =   -.89532( .00082)
D  =  -1.38361( .02438)
Atom              d          s           d/s      (d/s)**2
N1    *          .0233      .0043       5.431       29.490
N2    *         -.0228      .0042      -5.390       29.047
N3    *          .0167      .0043       3.910       15.286
N5    *         -.0260      .0053      -4.865       23.670
Cu1             -.2369      .0008    -289.170    83619.230
#===========
Sum((d/s)**2) for starred atoms       97.494
Chi-squared at 95% for  1 degrees of freedom:  3.84
The group of atoms deviates significantly from planarity


Plane  2
m1 =    .22662( .00105)
m2 =    .33244( .00139)
m3 =   -.91549( .00055)
D  =  -2.09307( .01627)
Atom              d          s           d/s      (d/s)**2
N1    *         -.0706      .0042     -16.635      276.733
N2    *         -.1153      .0042     -27.404      750.998
C7    *          .1073      .0071      15.122      228.669
C6    *          .1619      .0069      23.336      544.554
N3    *          .0710      .0042      16.799      282.202
N5    *          .0275      .0053       5.141       26.431
#===========
Sum((d/s)**2) for starred atoms     2109.585
Chi-squared at 95% for  3 degrees of freedom:  7.81
The group of atoms deviates significantly from planarity


Plane  3
m1 =    .13238( .00233)
m2 =    .31603( .00175)
m3 =   -.93947( .00071)
D  =  -3.52715( .03523)
Atom              d          s           d/s      (d/s)**2
N1    *          .0003      .0042        .072         .005
N2    *         -.0003      .0042       -.072         .005
C7    *          .0007      .0070        .095         .009
C6    *         -.0007      .0069       -.094         .009
#===========
Sum((d/s)**2) for starred atoms         .028
Chi-squared at 95% for  1 degrees of freedom:  3.84
The group of atoms does not deviate significantly from planarity


Plane  4
m1 =    .91102( .00087)
m2 =    .34077( .00197)
m3 =    .23221( .00278)
D  =  11.27695( .01204)
Atom              d          s           d/s      (d/s)**2
N3    *          .0000      .0049        .000         .000
N4    *          .0000      .0057        .000         .000
N5    *          .0000      .0052        .000         .000
#===========
Sum((d/s)**2) for starred atoms         .000

Plane  5
m1 =   -.92010( .00079)
m2 =   -.36215( .00185)
m3 =   -.14921( .00132)
D  = -10.87335( .00650)
Atom              d          s           d/s      (d/s)**2
N3    *         -.0718      .0049     -14.692      215.856
N4    *          .1228      .0057      21.523      463.229
N5    *         -.0796      .0052     -15.246      232.429
N6    *          .0827      .0062      13.347      178.141
#===========
Sum((d/s)**2) for starred atoms     1089.655
Chi-squared at 95% for  1 degrees of freedom:  3.84
The group of atoms deviates significantly from planarity


Plane  6
m1 =    .12090( .00342)
m2 =    .35786( .00358)
m3 =   -.92591( .00149)
D  =  -3.41877( .05410)
Atom              d          s           d/s      (d/s)**2
N1    *          .0000      .0042        .000         .000
C6    *          .0000      .0070        .000         .000
C4    *          .0000      .0070        .000         .000
#===========
Sum((d/s)**2) for starred atoms         .000

Plane  7
m1 =   -.15627( .00378)
m2 =   -.27665( .00306)
m3 =    .94818( .00097)
D  =   3.56026( .05001)
Atom              d          s           d/s      (d/s)**2
N2    *          .0000      .0041        .000         .000
C7    *          .0000      .0069        .000         .000
C9    *          .0000      .0068        .000         .000
#===========
Sum((d/s)**2) for starred atoms         .000

Weighted least-squares lines through the starred atoms
(Schoemaker,Waser,Marsh & Bergman,Acta Cryst.(1959).12,600)
m1,m2,m3 are the direction cosines referred to the X,Y,Z orthogonal axes.
X0,Y0,Z0 are the coordinates of the centroid of the set of atoms.
Equation of the line: (X-X0)/m1=(Y-Y0)/m2=(Z-Z0)/m3

Line  1
m1 =    .57956( .00216)     X0 =   9.62862( .00292)
m2 =    .40287( .00223)     Y0 =   3.88540( .00270)
m3 =   -.70838( .00172)     Z0 =   7.44067( .00270)
Atom              d          s           d/s      (d/s)**2
N4    *          .0000      .0078        .000         .000
Cu1   *          .0000      .0012        .003         .000
#===========
Sum((d/s)**2) for starred atoms         .000
Dihedral angles formed by LSQ-planes
Plane - plane            angle (s.u.)             angle (s.u.)
1       2               3.24(  .11)             176.76(  .11)
1       3               8.86(  .17)             171.14(  .17)
1       4              80.61(  .17)              99.39(  .17)
1       5              75.68(  .12)             104.32(  .12)
1       6               9.12(  .22)             170.88(  .22)
1       7               8.61(  .20)             171.39(  .20)
2       3               5.65(  .14)             174.35(  .14)
2       4              83.85(  .16)              96.15(  .16)
2       5              78.91(  .10)             101.09(  .10)
2       6               6.26(  .20)             173.74(  .20)
2       7               5.48(  .20)             174.52(  .20)
3       4              89.42(  .21)              90.58(  .21)
3       5              84.49(  .15)              95.51(  .15)
3       6               2.60(  .23)             177.40(  .23)
3       7               2.69(  .23)             177.31(  .23)
4       5               4.94(  .18)             175.06(  .18)
4       6              89.02(  .25)              90.98(  .25)
4       7              89.06(  .25)              90.94(  .25)
5       6              84.11(  .21)              95.89(  .21)
5       7              84.12(  .22)              95.88(  .22)
6       7               5.24(  .26)             174.76(  .26)

Angles formed by lines and normals to planes
Line  - plane            angle (s.u.)             angle (s.u.)
1       1              20.74(  .14)             159.26(  .14)
1       2              23.97(  .13)             156.03(  .13)
1       3              29.59(  .17)             150.41(  .17)
1       4              59.95(  .20)             120.05(  .20)
1       5              55.01(  .14)             124.99(  .14)
1       6              29.53(  .24)             150.47(  .24)
1       7              29.11(  .23)             150.89(  .23)
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 1.937(4) . ?
Cu1 N1 1.939(5) . ?
Cu1 N5 2.085(5) . ?
Cu1 N3 2.107(5) . ?
Cu1 N4 2.183(5) . ?
N1 C3 1.326(8) . ?
N1 C2 1.354(8) . ?
N2 C10 1.315(8) . ?
N2 C1 1.352(8) . ?
C1 C7 1.382(9) . ?
C1 C2 1.480(9) . ?
C2 C6 1.393(9) . ?
C3 C4 1.389(9) . ?
C3 C16 1.508(10) . ?
C4 C5 1.364(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.390(11) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.384(12) . ?
C7 H7 0.9300 . ?
C8 C9 1.380(11) . ?
C8 H8 0.9300 . ?
C9 C10 1.381(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.502(9) . ?
C11 N3 1.504(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
N3 C12 1.481(8) . ?
N3 C18 1.491(7) . ?
C12 C13 1.518(10) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N4 1.483(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N4 C14 1.487(9) . ?
N4 C17 1.478(8) . ?
C14 C15 1.515(10) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N5 1.502(8) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
N5 C23 1.487(8) . ?
N5 C16 1.518(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.517(8) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.511(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N6 1.494(9) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
N6 C21 1.508(9) . ?
N6 C24 1.514(8) . ?
N6 H100 0.70(5) . ?
C21 C22 1.514(9) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.516(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
Cl1 O12 1.360(10) . ?
Cl1 O12 1.360(10) 2_655 ?
Cl1 O13 1.403(12) . ?
Cl1 O13 1.403(12) 2_655 ?
Cl1 O11 1.395(9) . ?
Cl1 O14 1.526(13) . ?
Cl1 O14 1.526(13) 2_655 ?
O12 O13 1.150(19) . ?
O12 O14 1.36(2) . ?
O13 O14 1.71(2) 2_655 ?
O14 O13 1.71(2) 2_655 ?
Cl2 O21 1.381(6) . ?
Cl2 O21 1.381(6) 2_656 ?
Cl2 O22 1.393(8) 2_656 ?
Cl2 O22 1.393(8) . ?
Cl3 O34 1.216(15) . ?
Cl3 O33 1.302(10) . ?
Cl3 O31 1.347(7) . ?
Cl3 O32 1.381(7) . ?
Cl4 O44 1.237(9) . ?
Cl4 O43 1.330(12) . ?
Cl4 O42 1.382(8) . ?
Cl4 O41 1.419(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cu1 N1 80.6(2) . . ?
N2 Cu1 N5 160.4(2) . . ?
N1 Cu1 N5 82.5(2) . . ?
N2 Cu1 N3 81.59(19) . . ?
N1 Cu1 N3 158.0(2) . . ?
N5 Cu1 N3 112.15(19) . . ?
N2 Cu1 N4 110.5(2) . . ?
N1 Cu1 N4 114.2(2) . . ?
N5 Cu1 N4 85.65(19) . . ?
N3 Cu1 N4 84.1(2) . . ?
C3 N1 C2 122.3(5) . . ?
C3 N1 Cu1 120.0(4) . . ?
C2 N1 Cu1 117.7(4) . . ?
C10 N2 C1 122.6(5) . . ?
C10 N2 Cu1 120.3(4) . . ?
C1 N2 Cu1 117.1(4) . . ?
N2 C1 C7 120.0(6) . . ?
N2 C1 C2 112.9(5) . . ?
C7 C1 C2 127.1(6) . . ?
N1 C2 C6 119.3(6) . . ?
N1 C2 C1 111.7(5) . . ?
C6 C2 C1 129.0(6) . . ?
N1 C3 C4 120.5(7) . . ?
N1 C3 C16 114.0(5) . . ?
C4 C3 C16 125.4(6) . . ?
C5 C4 C3 118.5(7) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 121.2(6) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C2 C6 C5 118.1(7) . . ?
C2 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
C8 C7 C1 117.1(7) . . ?
C8 C7 H7 121.4 . . ?
C1 C7 H7 121.4 . . ?
C7 C8 C9 122.1(7) . . ?
C7 C8 H8 119.0 . . ?
C9 C8 H8 119.0 . . ?
C10 C9 C8 117.5(7) . . ?
C10 C9 H9 121.2 . . ?
C8 C9 H9 121.2 . . ?
N2 C10 C9 120.6(6) . . ?
N2 C10 C11 114.6(5) . . ?
C9 C10 C11 124.7(6) . . ?
C10 C11 N3 111.9(5) . . ?
C10 C11 H11A 109.2 . . ?
N3 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
N3 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C12 N3 C18 110.0(5) . . ?
C12 N3 C11 110.8(5) . . ?
C18 N3 C11 110.2(5) . . ?
C12 N3 Cu1 105.7(4) . . ?
C18 N3 Cu1 112.7(3) . . ?
C11 N3 Cu1 107.4(3) . . ?
N3 C12 C13 112.6(5) . . ?
N3 C12 H12A 109.1 . . ?
C13 C12 H12A 109.1 . . ?
N3 C12 H12B 109.1 . . ?
C13 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
N4 C13 C12 112.9(5) . . ?
N4 C13 H13A 109.0 . . ?
C12 C13 H13A 109.0 . . ?
N4 C13 H13B 109.0 . . ?
C12 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C13 N4 C14 114.3(6) . . ?
C13 N4 C17 109.1(6) . . ?
C14 N4 C17 109.1(6) . . ?
C13 N4 Cu1 107.1(4) . . ?
C14 N4 Cu1 104.6(4) . . ?
C17 N4 Cu1 112.8(4) . . ?
N4 C14 C15 111.5(5) . . ?
N4 C14 H14A 109.3 . . ?
C15 C14 H14A 109.3 . . ?
N4 C14 H14B 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
N5 C15 C14 111.8(6) . . ?
N5 C15 H15A 109.3 . . ?
C14 C15 H15A 109.3 . . ?
N5 C15 H15B 109.3 . . ?
C14 C15 H15B 109.3 . . ?
H15A C15 H15B 107.9 . . ?
C23 N5 C15 110.1(5) . . ?
C23 N5 C16 109.9(5) . . ?
C15 N5 C16 110.1(5) . . ?
C23 N5 Cu1 114.0(4) . . ?
C15 N5 Cu1 105.1(4) . . ?
C16 N5 Cu1 107.5(4) . . ?
C3 C16 N5 112.1(5) . . ?
C3 C16 H16A 109.2 . . ?
N5 C16 H16A 109.2 . . ?
C3 C16 H16B 109.2 . . ?
N5 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
N4 C17 H17A 109.5 . . ?
N4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 C19 112.3(5) . . ?
N3 C18 H18A 109.1 . . ?
C19 C18 H18A 109.1 . . ?
N3 C18 H18B 109.1 . . ?
C19 C18 H18B 109.1 . . ?
H18A C18 H18B 107.9 . . ?
C20 C19 C18 114.2(5) . . ?
C20 C19 H19A 108.7 . . ?
C18 C19 H19A 108.7 . . ?
C20 C19 H19B 108.7 . . ?
C18 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
N6 C20 C19 116.9(5) . . ?
N6 C20 H20A 108.1 . . ?
C19 C20 H20A 108.1 . . ?
N6 C20 H20B 108.1 . . ?
C19 C20 H20B 108.1 . . ?
H20A C20 H20B 107.3 . . ?
C20 N6 C21 118.0(6) . . ?
C20 N6 C24 108.7(6) . . ?
C21 N6 C24 107.0(6) . . ?
C20 N6 H100 113(4) . . ?
C21 N6 H100 110(4) . . ?
C24 N6 H100 98(4) . . ?
N6 C21 C22 117.5(5) . . ?
N6 C21 H21A 107.9 . . ?
C22 C21 H21A 107.9 . . ?
N6 C21 H21B 107.9 . . ?
C22 C21 H21B 107.9 . . ?
H21A C21 H21B 107.2 . . ?
C21 C22 C23 115.3(6) . . ?
C21 C22 H22A 108.4 . . ?
C23 C22 H22A 108.4 . . ?
C21 C22 H22B 108.4 . . ?
C23 C22 H22B 108.4 . . ?
H22A C22 H22B 107.5 . . ?
N5 C23 C22 112.9(5) . . ?
N5 C23 H23A 109.0 . . ?
C22 C23 H23A 109.0 . . ?
N5 C23 H23B 109.0 . . ?
C22 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
N6 C24 H24A 109.5 . . ?
N6 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N6 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O12 Cl1 O12 111.8(12) . 2_655 ?
O12 Cl1 O13 49.2(9) . . ?
O12 Cl1 O13 114.0(10) 2_655 . ?
O12 Cl1 O13 114.0(10) . 2_655 ?
O12 Cl1 O13 49.2(9) 2_655 2_655 ?
O13 Cl1 O13 154.6(13) . 2_655 ?
O12 Cl1 O11 124.1(6) . . ?
O12 Cl1 O11 124.1(6) 2_655 . ?
O13 Cl1 O11 102.7(7) . . ?
O13 Cl1 O11 102.7(7) 2_655 . ?
O12 Cl1 O14 55.9(10) . . ?
O12 Cl1 O14 107.8(10) 2_655 . ?
O13 Cl1 O14 102.7(10) . . ?
O13 Cl1 O14 71.4(9) 2_655 . ?
O11 Cl1 O14 103.1(6) . . ?
O12 Cl1 O14 107.8(10) . 2_655 ?
O12 Cl1 O14 55.9(10) 2_655 2_655 ?
O13 Cl1 O14 71.4(9) . 2_655 ?
O13 Cl1 O14 102.7(10) 2_655 2_655 ?
O11 Cl1 O14 103.1(6) . 2_655 ?
O14 Cl1 O14 153.8(13) . 2_655 ?
O13 O12 O14 131.2(15) . . ?
O13 O12 Cl1 67.4(9) . . ?
O14 O12 Cl1 68.2(9) . . ?
O12 O13 Cl1 63.4(8) . . ?
O12 O13 O14 107.6(12) . 2_655 ?
Cl1 O13 O14 57.7(7) . 2_655 ?
O12 O14 Cl1 55.8(7) . . ?
O12 O14 O13 97.2(10) . 2_655 ?
Cl1 O14 O13 51.0(6) . 2_655 ?
O21 Cl2 O21 115.5(7) . 2_656 ?
O21 Cl2 O22 108.0(5) . 2_656 ?
O21 Cl2 O22 107.0(5) 2_656 2_656 ?
O21 Cl2 O22 107.0(5) . . ?
O21 Cl2 O22 108.0(5) 2_656 . ?
O22 Cl2 O22 111.4(11) 2_656 . ?
O34 Cl3 O33 107.4(18) . . ?
O34 Cl3 O31 106.8(14) . . ?
O33 Cl3 O31 111.0(9) . . ?
O34 Cl3 O32 108.8(14) . . ?
O33 Cl3 O32 109.8(7) . . ?
O31 Cl3 O32 112.9(6) . . ?
O44 Cl4 O43 105.5(15) . . ?
O44 Cl4 O42 118.7(11) . . ?
O43 Cl4 O42 105.9(9) . . ?
O44 Cl4 O41 114.8(12) . . ?
O43 Cl4 O41 102.7(9) . . ?
O42 Cl4 O41 107.5(6) . . ?

_diffrn_measured_fraction_theta_max    0.920
_diffrn_reflns_theta_full              60.83
_diffrn_measured_fraction_theta_full   0.920
_refine_diff_density_max    0.786
_refine_diff_density_min   -0.891
_refine_diff_density_rms    0.093



#===END


data_[CuL1](ClO4)2
_database_code_CSD                  177617

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety
;
(C17 H23 N5 Cu 2+), (Cl O4 1-)2
;
_chemical_formula_sum
'C17 H23 Cl2 Cu N5 O8'
_chemical_formula_weight          559.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C'  'C'   0.0181   0.0091
'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'   0.0311   0.0180
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O'  'O'   0.0492   0.0322
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl'  'Cl'   0.3639   0.7018
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cu'  'Cu'  -1.9646   0.5888
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P21/c

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                    12.1570(10)
_cell_length_b                    8.8210(10)
_cell_length_c                    20.685(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  100.973(9)
_cell_angle_gamma                 90.00
_cell_volume                      2177.6(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     298
_cell_measurement_reflns_used     22
_cell_measurement_theta_min       12
_cell_measurement_theta_max       42

_exptl_crystal_description        prismatic
_exptl_crystal_colour             blue
_exptl_crystal_size_max           0.3
_exptl_crystal_size_mid           0.3
_exptl_crystal_size_min           0.2
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.708
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1148
_exptl_absorpt_coefficient_mu     4.186
_exptl_absorpt_correction_type    'empirical'
_exptl_absorpt_correction_T_min   0.27
_exptl_absorpt_correction_T_max   0.42
_exptl_absorpt_process_details    'PSI-scan'

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       298
_diffrn_radiation_wavelength      1.54180
_diffrn_radiation_type            CuK\a
_diffrn_radiation_source          'rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'SIEMENS P4'
_diffrn_measurement_method        '\q/2\q'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          3
_diffrn_standards_interval_count  200
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0
_diffrn_reflns_number             4100
_diffrn_reflns_av_R_equivalents   0.0743
_diffrn_reflns_av_sigmaI/netI     0.0561
_diffrn_reflns_limit_h_min        -1
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -1
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -23
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          3.70
_diffrn_reflns_theta_max          59.99
_reflns_number_total              3034
_reflns_number_gt                 2568
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'XSCANS-Bruker'
_computing_cell_refinement        'XSCANS-Bruker'
_computing_data_reduction         'XSCANS-Bruker'
_computing_structure_solution     'SIR97 (Altomare, 1999)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 (Ver. 1.01\b) (Farrugia, 1997)'
_computing_publication_material   'Parst97 (Nardelli, 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^)+(0.1214P)^2^+4.0446P] 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
_atom_sites_solution_H1N3         geom
_refine_ls_H1N3_treatment         refall
_atom_sites_solution_H1N5         geom
_refine_ls_H1N5_treatment         refall
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0058(6)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          3034
_refine_ls_number_parameters      308
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0773
_refine_ls_R_factor_gt            0.0684
_refine_ls_wR_factor_ref          0.2012
_refine_ls_wR_factor_gt           0.1885
_refine_ls_goodness_of_fit_ref    1.062
_refine_ls_restrained_S_all       1.062
_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
Cu1 Cu 0.73805(6) 0.10878(9) 0.12495(3) 0.0417(4) Uani 1 1 d . . .
N1 N 0.7006(4) 0.0544(5) 0.0317(2) 0.0463(11) Uani 1 1 d . . .
N2 N 0.5948(3) 0.2115(5) 0.09951(19) 0.0420(10) Uani 1 1 d . . .
C1 C 0.7635(5) -0.0448(7) 0.0066(3) 0.0509(14) Uani 1 1 d . . .
C2 C 0.7389(6) -0.0702(8) -0.0624(3) 0.0662(19) Uani 1 1 d . . .
H2 H 0.7806 -0.1401 -0.0813 0.079 Uiso 1 1 calc R . .
C3 C 0.6546(7) 0.0073(8) -0.1007(3) 0.069(2) Uani 1 1 d . . .
H3 H 0.6409 -0.0067 -0.1461 0.083 Uiso 1 1 calc R . .
C4 C 0.5890(6) 0.1066(7) -0.0733(3) 0.0562(16) Uani 1 1 d . . .
H4 H 0.5297 0.1578 -0.0993 0.067 Uiso 1 1 calc R . .
C5 C 0.6143(5) 0.1277(6) -0.0057(2) 0.0454(13) Uani 1 1 d . . .
C6 C 0.5523(4) 0.2247(6) 0.0345(2) 0.0439(13) Uani 1 1 d . . .
C7 C 0.4589(5) 0.3138(8) 0.0132(3) 0.0568(15) Uani 1 1 d . . .
H7 H 0.4280 0.3224 -0.0314 0.068 Uiso 1 1 calc R . .
C8 C 0.4122(5) 0.3904(7) 0.0606(3) 0.0590(16) Uani 1 1 d . . .
H8 H 0.3502 0.4525 0.0474 0.071 Uiso 1 1 calc R . .
C9 C 0.4572(5) 0.3750(7) 0.1267(3) 0.0533(15) Uani 1 1 d . . .
H9 H 0.4257 0.4260 0.1581 0.064 Uiso 1 1 calc R . .
C10 C 0.5492(4) 0.2831(6) 0.1456(3) 0.0433(12) Uani 1 1 d . . .
C11 C 0.6085(5) 0.2446(7) 0.2140(3) 0.0493(14) Uani 1 1 d . . .
H11A H 0.6052 0.3303 0.2429 0.059 Uiso 1 1 calc R . .
H11B H 0.5718 0.1593 0.2305 0.059 Uiso 1 1 calc R . .
N3 N 0.7274(4) 0.2059(6) 0.2137(2) 0.0453(11) Uani 1 1 d . . .
H1N3 H 0.755(6) 0.145(8) 0.249(3) 0.056(18) Uiso 1 1 d . . .
C12 C 0.7948(5) 0.3471(7) 0.2207(3) 0.0499(14) Uani 1 1 d . . .
H12A H 0.8111 0.3773 0.2666 0.060 Uiso 1 1 calc R . .
H12B H 0.7518 0.4276 0.1957 0.060 Uiso 1 1 calc R . .
C13 C 0.9045(5) 0.3254(8) 0.1962(3) 0.0529(14) Uani 1 1 d . . .
H13A H 0.9449 0.4206 0.1986 0.063 Uiso 1 1 calc R . .
H13B H 0.9512 0.2520 0.2237 0.063 Uiso 1 1 calc R . .
N4 N 0.8789(4) 0.2711(6) 0.1272(2) 0.0453(11) Uani 1 1 d . . .
C14 C 0.8495(6) 0.4019(7) 0.0815(3) 0.0584(16) Uani 1 1 d . . .
H14A H 0.7886 0.4575 0.0935 0.088 Uiso 1 1 calc R . .
H14B H 0.8276 0.3651 0.0372 0.088 Uiso 1 1 calc R . .
H14C H 0.9134 0.4672 0.0842 0.088 Uiso 1 1 calc R . .
C15 C 0.9719(5) 0.1837(8) 0.1100(3) 0.0575(15) Uani 1 1 d . . .
H15A H 1.0419 0.2363 0.1257 0.069 Uiso 1 1 calc R . .
H15B H 0.9618 0.1744 0.0625 0.069 Uiso 1 1 calc R . .
C16 C 0.9764(5) 0.0269(8) 0.1409(3) 0.0594(16) Uani 1 1 d . . .
H16A H 1.0343 -0.0326 0.1264 0.071 Uiso 1 1 calc R . .
H16B H 0.9954 0.0359 0.1884 0.071 Uiso 1 1 calc R . .
N5 N 0.8676(4) -0.0509(7) 0.1221(3) 0.0560(13) Uani 1 1 d . . .
H1N5 H 0.859(6) -0.119(8) 0.142(3) 0.06(2) Uiso 1 1 d . . .
C17 C 0.8492(6) -0.1245(8) 0.0553(4) 0.0691(19) Uani 1 1 d . . .
H17A H 0.9194 -0.1259 0.0395 0.083 Uiso 1 1 calc R . .
H17B H 0.8258 -0.2287 0.0592 0.083 Uiso 1 1 calc R . .
Cl2 Cl 0.68411(12) -0.25423(16) 0.21178(7) 0.0548(5) Uani 1 1 d . . .
O21 O 0.6352(6) -0.3529(7) 0.2505(4) 0.115(2) Uani 1 1 d . . .
O22 O 0.6714(7) -0.3133(9) 0.1466(3) 0.127(3) Uani 1 1 d . . .
O23 O 0.6345(7) -0.1094(6) 0.2071(4) 0.108(2) Uani 1 1 d . . .
O24 O 0.7982(5) -0.2509(11) 0.2342(4) 0.144(3) Uani 1 1 d . . .
Cl1 Cl 0.84655(12) 0.38305(18) -0.11152(6) 0.0546(5) Uani 1 1 d . . .
O11 O 0.7316(4) 0.3565(6) -0.1405(2) 0.0744(14) Uani 1 1 d . . .
O12 O 0.8561(4) 0.5218(6) -0.0760(2) 0.0772(14) Uani 1 1 d . . .
O13 O 0.9125(5) 0.3840(8) -0.1620(3) 0.105(2) Uani 1 1 d . . .
O14 O 0.8811(5) 0.2593(7) -0.0668(2) 0.0944(18) Uani 1 1 d . . .

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
Cu1 0.0444(5) 0.0482(6) 0.0349(5) -0.0025(3) 0.0140(3) 0.0027(3)
N1 0.050(3) 0.049(3) 0.044(2) -0.008(2) 0.018(2) -0.005(2)
N2 0.044(2) 0.048(3) 0.036(2) -0.0036(19) 0.0111(18) -0.004(2)
C1 0.057(3) 0.051(3) 0.053(3) -0.013(3) 0.030(3) -0.011(3)
C2 0.084(5) 0.064(4) 0.064(4) -0.023(4) 0.050(4) -0.022(4)
C3 0.096(5) 0.075(5) 0.041(3) -0.017(3) 0.025(3) -0.032(4)
C4 0.068(4) 0.062(4) 0.040(3) -0.005(3) 0.014(3) -0.021(3)
C5 0.054(3) 0.050(3) 0.035(3) -0.001(2) 0.016(2) -0.014(3)
C6 0.041(3) 0.053(3) 0.039(3) 0.002(2) 0.013(2) -0.011(2)
C7 0.050(3) 0.065(4) 0.051(3) 0.011(3) 0.000(3) -0.004(3)
C8 0.049(3) 0.056(4) 0.074(4) 0.009(3) 0.017(3) 0.010(3)
C9 0.052(3) 0.051(3) 0.062(4) -0.004(3) 0.026(3) 0.006(3)
C10 0.046(3) 0.042(3) 0.045(3) -0.001(2) 0.020(2) -0.004(2)
C11 0.056(3) 0.052(3) 0.045(3) -0.005(3) 0.023(3) 0.001(3)
N3 0.052(3) 0.051(3) 0.035(2) 0.002(2) 0.015(2) 0.002(2)
C12 0.059(3) 0.054(3) 0.039(3) -0.007(3) 0.015(2) -0.014(3)
C13 0.055(3) 0.066(4) 0.038(3) -0.001(3) 0.009(2) -0.008(3)
N4 0.047(2) 0.058(3) 0.034(2) 0.002(2) 0.0156(19) 0.001(2)
C14 0.070(4) 0.054(4) 0.053(3) 0.010(3) 0.017(3) -0.001(3)
C15 0.056(3) 0.066(4) 0.056(3) -0.001(3) 0.025(3) 0.005(3)
C16 0.051(3) 0.068(4) 0.061(4) 0.010(3) 0.013(3) 0.008(3)
N5 0.061(3) 0.051(3) 0.061(3) 0.010(3) 0.026(3) 0.005(3)
C17 0.069(4) 0.066(4) 0.079(5) -0.016(4) 0.031(4) 0.008(3)
Cl2 0.0661(10) 0.0526(9) 0.0498(8) 0.0069(6) 0.0214(7) 0.0025(7)
O21 0.149(6) 0.086(4) 0.138(5) 0.047(4) 0.100(5) 0.013(4)
O22 0.201(8) 0.119(5) 0.058(3) -0.013(3) 0.015(4) 0.030(6)
O23 0.141(6) 0.054(3) 0.128(5) 0.002(3) 0.023(4) 0.021(3)
O24 0.074(4) 0.162(7) 0.180(7) 0.064(6) -0.012(4) -0.010(4)
Cl1 0.0555(9) 0.0719(10) 0.0399(8) -0.0060(6) 0.0176(6) -0.0024(7)
O11 0.062(3) 0.096(4) 0.066(3) -0.009(3) 0.016(2) -0.003(3)
O12 0.095(3) 0.071(3) 0.071(3) -0.017(3) 0.028(3) -0.015(3)
O13 0.093(4) 0.164(6) 0.075(3) -0.041(4) 0.054(3) -0.056(4)
O14 0.121(5) 0.094(4) 0.066(3) 0.004(3) 0.010(3) 0.036(4)

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

Weighted least-squares planes through the starred atoms
(Nardelli, Musatti, Domiano & Andreetti Ric.Sci.(1965),15(II-A),807).
Equation of the plane: m1*X+m2*Y+m3*Z=d

Plane  1
m1 =    .58486( .00146)
m2 =    .78002( .00104)
m3 =   -.22251( .00186)
D  =   5.06664( .01308)
Atom              d          s           d/s      (d/s)**2
N1    *          .0728      .0046      15.899      252.771
N2    *         -.0610      .0042     -14.667      215.127
N3    *          .0644      .0051      12.583      158.338
N5    *         -.0809      .0058     -13.962      194.932
Cu1              .0772      .0008     100.027    10005.430
#===========
Sum((d/s)**2) for starred atoms      821.168
Chi-squared at 95% for  1 degrees of freedom:  3.84
The group of atoms deviates significantly from planarity


Plane  2
m1 =    .61038( .00110)
m2 =    .77287( .00092)
m3 =   -.17350( .00128)
D  =   5.39980( .00818)
Atom              d          s           d/s      (d/s)**2
N1    *         -.0181      .0046      -3.924       15.398
N2    *         -.1339      .0042     -32.259     1040.618
C4    *          .1319      .0067      19.835      393.433
C7    *          .0665      .0067       9.901       98.030
N3    *          .1351      .0051      26.364      695.061
N5    *         -.0324      .0058      -5.627       31.665
#===========
Sum((d/s)**2) for starred atoms     2274.205
Chi-squared at 95% for  3 degrees of freedom:  7.81
The group of atoms deviates significantly from planarity


Plane  3
m1 =   -.63475( .00170)
m2 =    .05432( .00258)
m3 =   -.77080( .00137)
D  =  -8.32551( .01341)
Atom              d          s           d/s      (d/s)**2
N3    *          .0000      .0044        .000         .000
N4    *          .0000      .0044        .000         .000
N5    *          .0000      .0057        .000         .000
#===========
Sum((d/s)**2) for starred atoms         .000

Plane  4
m1 =   -.66255( .00315)
m2 =   -.73694( .00277)
m3 =    .13400( .00331)
D  =  -5.82773( .02524)
Atom              d          s           d/s      (d/s)**2
N1    *          .0000      .0046        .000         .000
C4    *          .0000      .0067        .000         .000
C2    *          .0000      .0072        .000         .000
#===========
Sum((d/s)**2) for starred atoms         .000

Plane  5
m1 =    .61748( .00254)
m2 =    .78441( .00204)
m3 =   -.05850( .00346)
D  =   5.56832( .01283)
Atom              d          s           d/s      (d/s)**2
N2    *          .0000      .0042        .000         .000
C7    *          .0000      .0067        .000         .000
C9    *          .0000      .0062        .000         .000
#===========
Sum((d/s)**2) for starred atoms         .000

Weighted least-squares lines through the starred atoms
(Schoemaker,Waser,Marsh & Bergman,Acta Cryst.(1959).12,600)
m1,m2,m3 are the direction cosines referred to the X,Y,Z orthogonal axes.
X0,Y0,Z0 are the coordinates of the centroid of the set of atoms.
Equation of the line: (X-X0)/m1=(Y-Y0)/m2=(Z-Z0)/m3

Line  1
m1 =   -.76534( .00149)     X0 =   9.33237( .00249)
m2 =   -.64330( .00178)     Y0 =   1.67546( .00268)
m3 =   -.02053( .00185)     Z0 =   2.56021( .00205)
Atom              d          s           d/s      (d/s)**2
N4    *          .0000      .0066        .000         .000
Cu1   *          .0000      .0010        .002         .000
#===========
Sum((d/s)**2) for starred atoms         .000
Dihedral angles formed by LSQ-planes
Plane - plane            angle (s.u.)             angle (s.u.)
1       2               3.19(  .12)             176.81(  .12)
1       3              80.95(  .16)              99.05(  .16)
1       4               7.19(  .21)             172.81(  .21)
1       5               9.60(  .22)             170.40(  .22)
2       3              77.78(  .15)             102.22(  .15)
2       4               4.28(  .19)             175.72(  .19)
2       5               6.64(  .22)             173.36(  .22)
3       4              73.90(  .23)             106.10(  .23)
3       5              72.29(  .24)             107.71(  .24)
4       5               5.73(  .26)             174.27(  .26)

Angles formed by lines and normals to planes
Line  - plane            angle (s.u.)             angle (s.u.)
1       1              19.12(  .13)             160.88(  .13)
1       2              16.10(  .12)             163.90(  .12)
1       3              62.18(  .17)             117.82(  .17)
1       4              11.93(  .19)             168.07(  .19)
1       5              12.58(  .18)             167.42(  .18)


;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 1.945(4) . ?
Cu1 N1 1.956(4) . ?
Cu1 N3 2.053(4) . ?
Cu1 N5 2.122(5) . ?
Cu1 N4 2.226(5) . ?
N1 C1 1.330(7) . ?
N1 C5 1.344(7) . ?
N2 C10 1.348(7) . ?
N2 C6 1.351(6) . ?
C1 C2 1.419(9) . ?
C1 C17 1.482(10) . ?
C2 C3 1.355(11) . ?
C2 H2 0.9300 . ?
C3 C4 1.377(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.492(8) . ?
C6 C7 1.382(8) . ?
C7 C8 1.396(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.381(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.377(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.499(8) . ?
C11 N3 1.486(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
N3 C12 1.483(7) . ?
N3 H1N3 0.92(7) . ?
C12 C13 1.526(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N4 1.481(7) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N4 C15 1.467(7) . ?
N4 C14 1.492(7) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.520(9) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N5 1.474(9) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
N5 C17 1.505(9) . ?
N5 H1N5 0.75(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
Cl2 O24 1.377(6) . ?
Cl2 O21 1.390(5) . ?
Cl2 O23 1.408(6) . ?
Cl2 O22 1.426(6) . ?
Cl1 O12 1.421(5) . ?
Cl1 O11 1.431(5) . ?
Cl1 O13 1.433(5) . ?
Cl1 O14 1.440(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cu1 N1 79.57(18) . . ?
N2 Cu1 N3 80.92(18) . . ?
N1 Cu1 N3 160.5(2) . . ?
N2 Cu1 N5 158.9(2) . . ?
N1 Cu1 N5 81.1(2) . . ?
N3 Cu1 N5 118.4(2) . . ?
N2 Cu1 N4 110.60(18) . . ?
N1 Cu1 N4 102.27(17) . . ?
N3 Cu1 N4 83.78(17) . . ?
N5 Cu1 N4 81.7(2) . . ?
C1 N1 C5 122.4(5) . . ?
C1 N1 Cu1 120.2(4) . . ?
C5 N1 Cu1 117.3(4) . . ?
C10 N2 C6 122.2(5) . . ?
C10 N2 Cu1 119.6(3) . . ?
C6 N2 Cu1 117.5(3) . . ?
N1 C1 C2 118.0(6) . . ?
N1 C1 C17 115.4(5) . . ?
C2 C1 C17 126.5(6) . . ?
C3 C2 C1 119.9(6) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 120.9(6) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C3 C4 C5 117.7(6) . . ?
C3 C4 H4 121.1 . . ?
C5 C4 H4 121.1 . . ?
N1 C5 C4 121.0(5) . . ?
N1 C5 C6 112.2(4) . . ?
C4 C5 C6 126.8(6) . . ?
N2 C6 C7 120.1(5) . . ?
N2 C6 C5 111.5(5) . . ?
C7 C6 C5 128.3(5) . . ?
C6 C7 C8 118.1(5) . . ?
C6 C7 H7 120.9 . . ?
C8 C7 H7 120.9 . . ?
C9 C8 C7 120.7(6) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C10 C9 C8 119.1(5) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
N2 C10 C9 119.8(5) . . ?
N2 C10 C11 111.9(5) . . ?
C9 C10 C11 128.3(5) . . ?
N3 C11 C10 110.0(4) . . ?
N3 C11 H11A 109.7 . . ?
C10 C11 H11A 109.7 . . ?
N3 C11 H11B 109.7 . . ?
C10 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C12 N3 C11 109.0(5) . . ?
C12 N3 Cu1 108.0(3) . . ?
C11 N3 Cu1 109.0(3) . . ?
C12 N3 H1N3 108(4) . . ?
C11 N3 H1N3 110(4) . . ?
Cu1 N3 H1N3 113(4) . . ?
N3 C12 C13 111.3(5) . . ?
N3 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
N3 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
N4 C13 C12 108.9(4) . . ?
N4 C13 H13A 109.9 . . ?
C12 C13 H13A 109.9 . . ?
N4 C13 H13B 109.9 . . ?
C12 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C15 N4 C13 111.9(5) . . ?
C15 N4 C14 110.8(4) . . ?
C13 N4 C14 110.1(5) . . ?
C15 N4 Cu1 106.4(4) . . ?
C13 N4 Cu1 104.4(3) . . ?
C14 N4 Cu1 113.2(4) . . ?
N4 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 C16 110.2(5) . . ?
N4 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
N4 C15 H15B 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
N5 C16 C15 110.7(5) . . ?
N5 C16 H16A 109.5 . . ?
C15 C16 H16A 109.5 . . ?
N5 C16 H16B 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
C16 N5 C17 114.3(5) . . ?
C16 N5 Cu1 108.5(4) . . ?
C17 N5 Cu1 109.3(4) . . ?
C16 N5 H1N5 116(6) . . ?
C17 N5 H1N5 99(5) . . ?
Cu1 N5 H1N5 109(6) . . ?
C1 C17 N5 112.4(5) . . ?
C1 C17 H17A 109.1 . . ?
N5 C17 H17A 109.1 . . ?
C1 C17 H17B 109.1 . . ?
N5 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
O24 Cl2 O21 109.5(5) . . ?
O24 Cl2 O23 113.3(5) . . ?
O21 Cl2 O23 112.5(4) . . ?
O24 Cl2 O22 104.3(6) . . ?
O21 Cl2 O22 109.5(5) . . ?
O23 Cl2 O22 107.4(4) . . ?
O12 Cl1 O11 109.5(3) . . ?
O12 Cl1 O13 111.7(3) . . ?
O11 Cl1 O13 109.5(3) . . ?
O12 Cl1 O14 109.6(3) . . ?
O11 Cl1 O14 106.7(4) . . ?
O13 Cl1 O14 109.7(4) . . ?

_diffrn_measured_fraction_theta_max    0.939
_diffrn_reflns_theta_full              59.99
_diffrn_measured_fraction_theta_full   0.939
_refine_diff_density_max    0.674
_refine_diff_density_min   -0.776
_refine_diff_density_rms    0.097

#===END