# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2002

data_global

_journal_coden_Cambridge      440

_publ_requested_journal       'New Journal of Chemistry'

loop_
_publ_author_name
'Perez, Jose'
'Garcia, Luis'
'Garcia, Gabriel'
'Orpen, A. Guy'
'Saez, Paloma'
'Santana, M. Dolores'

_publ_contact_author_name     	'Dr Jose Perez'  
_publ_contact_author_address 
;
Ingenieria Minera, Geologica y Cartografica
Universidad Politecnica de Cartagena
Area de Quimica Inorgania.Campus Mu
Cartagena
Murcia
30202
SPAIN
;

_publ_contact_author_email       'JOSE.PPEREZ@UPCT.ES'

_publ_section_title		
;
Conformational analysis of complexes of
2,4,4-trimethyl-1,5,9-triazacyclododec-1-ene or its 9-methyl derivative
;

data_l1py 

_database_code_CSD	182499


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C17 H28 Cl2 N4 Ni O5' 
_chemical_formula_weight          498.04 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0033   0.0016 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0106   0.0060 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Cl'  'Cl'   0.1484   0.1585 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Ni'  'Ni'   0.3393   1.1124 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 

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                    13.4121(8) 
_cell_length_b                    9.0913(5) 
_cell_length_c                    18.3528(12) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  104.904(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      2162.5(2) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     81 
_cell_measurement_theta_min       5.547 
_cell_measurement_theta_max       12.309 

_exptl_crystal_description        block 
_exptl_crystal_colour             blue 
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.30 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.530 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1040 
_exptl_absorpt_coefficient_mu     1.180 
_exptl_absorpt_correction_type    non 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             7575 
_diffrn_reflns_av_R_equivalents   0.0387 
_diffrn_reflns_av_sigmaI/netI     0.0524 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          3.10 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              3794 
_reflns_number_gt                 2736 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_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^)+(0.0742P)^2^+0.0000P] 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          3794 
_refine_ls_number_parameters      262 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0594 
_refine_ls_R_factor_gt            0.0384 
_refine_ls_wR_factor_ref          0.1150 
_refine_ls_wR_factor_gt           0.0965 
_refine_ls_goodness_of_fit_ref    0.930 
_refine_ls_restrained_S_all       0.930 
_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 
Ni1 Ni 0.21330(3) 0.79761(5) 0.11068(2) 0.02461(15) Uani 1 1 d . . . 
Cl1 Cl 0.44945(7) 0.57908(13) 0.07625(6) 0.0477(3) Uani 1 1 d . . . 
N4 N 0.2522(2) 0.6159(3) 0.05267(16) 0.0260(7) Uani 1 1 d . . . 
O1 O 0.0905(2) 0.6786(3) 0.04546(15) 0.0377(7) Uani 1 1 d . . . 
C15 C 0.1958(3) 0.4282(4) -0.0686(2) 0.0341(9) Uani 1 1 d . . . 
H15 H 0.1773 0.3657 -0.1100 0.041 Uiso 1 1 calc R . . 
C17 C 0.3225(3) 0.5438(4) 0.0265(2) 0.0291(8) Uani 1 1 d . . . 
C16 C 0.2990(3) 0.4507(4) -0.0333(2) 0.0337(9) Uani 1 1 d . . . 
H16 H 0.3506 0.4036 -0.0500 0.040 Uiso 1 1 calc R . . 
C13 C 0.1502(3) 0.5968(4) 0.0180(2) 0.0294(8) Uani 1 1 d . . . 
C14 C 0.1208(3) 0.4976(4) -0.0428(2) 0.0345(9) Uani 1 1 d . . . 
H14 H 0.0514 0.4795 -0.0652 0.041 Uiso 1 1 calc R . . 
Cl2 Cl 0.70619(7) 0.84687(10) 0.20249(5) 0.0317(2) Uani 1 1 d . . . 
O4 O 0.7447(3) 0.7023(3) 0.22322(18) 0.0590(9) Uani 1 1 d . . . 
O3 O 0.7863(2) 0.9317(3) 0.18422(17) 0.0511(8) Uani 1 1 d . . . 
O5 O 0.6768(2) 0.9148(3) 0.26518(16) 0.0462(7) Uani 1 1 d . . . 
O2 O 0.6194(3) 0.8394(4) 0.13835(19) 0.0637(10) Uani 1 1 d . . . 
N3 N 0.2141(2) 0.7279(3) 0.21513(17) 0.0320(7) Uani 1 1 d . . . 
H3 H 0.2339 0.6319 0.2172 0.038 Uiso 1 1 calc R . . 
N2 N 0.3476(2) 0.9096(3) 0.12986(16) 0.0272(7) Uani 1 1 d . . . 
H2 H 0.3925 0.8479 0.1156 0.033 Uiso 1 1 calc R . . 
N1 N 0.1313(2) 0.9778(3) 0.11753(16) 0.0295(7) Uani 1 1 d . . . 
C2 C 0.2595(3) 1.1507(4) 0.0943(2) 0.0323(9) Uani 1 1 d . . . 
H2A H 0.3002 1.2014 0.1386 0.039 Uiso 1 1 calc R . . 
H2B H 0.2448 1.2219 0.0536 0.039 Uiso 1 1 calc R . . 
C5 C 0.3934(3) 0.8240(4) 0.2629(2) 0.0374(10) Uani 1 1 d . . . 
H5A H 0.4131 0.7339 0.2421 0.045 Uiso 1 1 calc R . . 
H5B H 0.4436 0.8421 0.3106 0.045 Uiso 1 1 calc R . . 
C3 C 0.3294(3) 1.0332(4) 0.0736(2) 0.0336(9) Uani 1 1 d . . . 
C6 C 0.2889(3) 0.8019(4) 0.2780(2) 0.0389(10) Uani 1 1 d . . . 
H6A H 0.2970 0.7436 0.3234 0.047 Uiso 1 1 calc R . . 
H6B H 0.2613 0.8969 0.2869 0.047 Uiso 1 1 calc R . . 
C4 C 0.3983(3) 0.9501(4) 0.2094(2) 0.0344(9) Uani 1 1 d . . . 
H4A H 0.3644 1.0357 0.2234 0.041 Uiso 1 1 calc R . . 
H4B H 0.4698 0.9754 0.2137 0.041 Uiso 1 1 calc R . . 
C7 C 0.1084(3) 0.7275(5) 0.2269(3) 0.0416(10) Uani 1 1 d . . . 
H7A H 0.1123 0.6941 0.2777 0.050 Uiso 1 1 calc R . . 
H7B H 0.0662 0.6578 0.1923 0.050 Uiso 1 1 calc R . . 
C1 C 0.1578(3) 1.1120(4) 0.1102(2) 0.0305(8) Uani 1 1 d . . . 
C9 C 0.0345(3) 0.9406(4) 0.1363(2) 0.0373(9) Uani 1 1 d . . . 
H9A H -0.0032 0.8690 0.1005 0.045 Uiso 1 1 calc R . . 
H9B H -0.0078 1.0281 0.1328 0.045 Uiso 1 1 calc R . . 
C10 C 0.0922(4) 1.2428(4) 0.1167(3) 0.0469(11) Uani 1 1 d . . . 
H10A H 0.0290 1.2100 0.1267 0.070 Uiso 1 1 calc R . . 
H10B H 0.0771 1.2974 0.0704 0.070 Uiso 1 1 calc R . . 
H10C H 0.1287 1.3047 0.1573 0.070 Uiso 1 1 calc R . . 
C11 C 0.2792(3) 0.9660(5) -0.0035(2) 0.0388(10) Uani 1 1 d . . . 
H11A H 0.2156 0.9191 -0.0020 0.058 Uiso 1 1 calc R . . 
H11B H 0.3249 0.8947 -0.0160 0.058 Uiso 1 1 calc R . . 
H11C H 0.2654 1.0422 -0.0410 0.058 Uiso 1 1 calc R . . 
C8 C 0.0558(3) 0.8782(5) 0.2152(2) 0.0435(10) Uani 1 1 d . . . 
H8A H -0.0092 0.8708 0.2290 0.052 Uiso 1 1 calc R . . 
H8B H 0.0988 0.9475 0.2497 0.052 Uiso 1 1 calc R . . 
C12 C 0.4308(3) 1.1067(5) 0.0711(2) 0.0452(11) Uani 1 1 d . . . 
H12A H 0.4760 1.0349 0.0582 0.068 Uiso 1 1 calc R . . 
H12B H 0.4629 1.1480 0.1196 0.068 Uiso 1 1 calc R . . 
H12C H 0.4174 1.1833 0.0339 0.068 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 0.0243(3) 0.0228(2) 0.0260(3) -0.00288(19) 0.00500(18) 0.00171(19) 
Cl1 0.0237(5) 0.0590(7) 0.0583(7) -0.0174(6) 0.0068(5) 0.0044(5) 
N4 0.0218(16) 0.0262(16) 0.0310(16) -0.0024(13) 0.0083(13) 0.0003(12) 
O1 0.0267(14) 0.0375(15) 0.0474(17) -0.0166(13) 0.0068(12) 0.0010(12) 
C15 0.044(2) 0.0262(19) 0.031(2) -0.0072(16) 0.0087(18) -0.0035(17) 
C17 0.0223(19) 0.0296(19) 0.037(2) 0.0022(16) 0.0109(16) 0.0006(15) 
C16 0.037(2) 0.0273(19) 0.041(2) -0.0023(17) 0.0175(19) 0.0019(16) 
C13 0.025(2) 0.0270(19) 0.035(2) -0.0005(16) 0.0070(16) 0.0011(15) 
C14 0.028(2) 0.029(2) 0.040(2) -0.0058(17) -0.0024(17) -0.0035(16) 
Cl2 0.0389(5) 0.0272(5) 0.0291(5) -0.0006(4) 0.0091(4) -0.0018(4) 
O4 0.105(3) 0.0301(16) 0.0519(19) 0.0065(14) 0.0381(19) 0.0174(17) 
O3 0.0526(19) 0.0541(19) 0.0475(18) 0.0006(15) 0.0146(15) -0.0184(16) 
O5 0.062(2) 0.0383(16) 0.0413(16) -0.0053(13) 0.0193(15) 0.0059(14) 
O2 0.048(2) 0.084(3) 0.050(2) -0.0183(18) -0.0040(16) -0.0074(18) 
N3 0.0399(19) 0.0228(16) 0.0346(17) 0.0018(13) 0.0121(15) 0.0023(13) 
N2 0.0295(17) 0.0235(15) 0.0278(16) -0.0029(13) 0.0058(13) 0.0021(13) 
N1 0.0318(17) 0.0284(17) 0.0265(16) 0.0007(13) 0.0045(14) 0.0056(13) 
C2 0.043(2) 0.0228(18) 0.031(2) 0.0043(15) 0.0101(18) 0.0022(16) 
C5 0.039(2) 0.036(2) 0.029(2) -0.0013(17) -0.0061(18) 0.0044(18) 
C3 0.044(2) 0.028(2) 0.027(2) 0.0008(16) 0.0054(17) -0.0027(17) 
C6 0.054(3) 0.035(2) 0.026(2) 0.0017(17) 0.0088(19) 0.003(2) 
C4 0.033(2) 0.035(2) 0.029(2) -0.0067(17) -0.0031(17) -0.0016(17) 
C7 0.042(2) 0.043(2) 0.048(3) 0.009(2) 0.027(2) 0.0021(19) 
C1 0.033(2) 0.033(2) 0.0250(19) 0.0015(16) 0.0071(16) 0.0093(17) 
C9 0.031(2) 0.033(2) 0.051(3) -0.0031(19) 0.0163(19) 0.0090(17) 
C10 0.056(3) 0.028(2) 0.053(3) 0.0007(19) 0.007(2) 0.015(2) 
C11 0.048(3) 0.041(2) 0.028(2) 0.0007(17) 0.0115(19) -0.0009(19) 
C8 0.045(3) 0.045(3) 0.048(3) 0.003(2) 0.026(2) 0.009(2) 
C12 0.052(3) 0.042(2) 0.046(3) 0.001(2) 0.021(2) -0.012(2) 

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

loop_ 
_geom_bond_atom_site_label_1 
_geom_bond_atom_site_label_2 
_geom_bond_distance 
_geom_bond_site_symmetry_2 
_geom_bond_publ_flag 
Ni1 N1 1.995(3) . ? 
Ni1 N3 2.017(3) . ? 
Ni1 N2 2.020(3) . ? 
Ni1 O1 2.074(3) . ? 
Ni1 N4 2.103(3) . ? 
Cl1 C17 1.743(4) . ? 
N4 C17 1.335(5) . ? 
N4 C13 1.364(4) . ? 
O1 C13 1.286(4) . ? 
C15 C14 1.372(5) . ? 
C15 C16 1.384(6) . ? 
C17 C16 1.357(5) . ? 
C13 C14 1.410(5) . ? 
Cl2 O4 1.428(3) . ? 
Cl2 O2 1.428(3) . ? 
Cl2 O3 1.431(3) . ? 
Cl2 O5 1.447(3) . ? 
N3 C6 1.481(5) . ? 
N3 C7 1.488(5) . ? 
N2 C4 1.489(4) . ? 
N2 C3 1.502(5) . ? 
N1 C1 1.288(5) . ? 
N1 C9 1.465(5) . ? 
C2 C1 1.508(5) . ? 
C2 C3 1.532(5) . ? 
C5 C6 1.511(6) . ? 
C5 C4 1.522(5) . ? 
C3 C12 1.527(6) . ? 
C3 C11 1.530(5) . ? 
C7 C8 1.531(6) . ? 
C1 C10 1.503(5) . ? 
C9 C8 1.513(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 
N1 Ni1 N3 93.81(12) . . ? 
N1 Ni1 N2 93.26(12) . . ? 
N3 Ni1 N2 101.91(12) . . ? 
N1 Ni1 O1 95.49(11) . . ? 
N3 Ni1 O1 101.18(12) . . ? 
N2 Ni1 O1 154.66(12) . . ? 
N1 Ni1 N4 152.84(12) . . ? 
N3 Ni1 N4 107.04(12) . . ? 
N2 Ni1 N4 99.08(11) . . ? 
O1 Ni1 N4 64.01(11) . . ? 
C17 N4 C13 119.1(3) . . ? 
C17 N4 Ni1 149.1(3) . . ? 
C13 N4 Ni1 89.2(2) . . ? 
C13 O1 Ni1 92.6(2) . . ? 
C14 C15 C16 120.3(4) . . ? 
N4 C17 C16 124.0(3) . . ? 
N4 C17 Cl1 114.0(3) . . ? 
C16 C17 Cl1 122.0(3) . . ? 
C17 C16 C15 117.8(4) . . ? 
O1 C13 N4 113.2(3) . . ? 
O1 C13 C14 127.2(3) . . ? 
N4 C13 C14 119.5(3) . . ? 
C15 C14 C13 119.2(3) . . ? 
O4 Cl2 O2 109.7(2) . . ? 
O4 Cl2 O3 108.5(2) . . ? 
O2 Cl2 O3 109.5(2) . . ? 
O4 Cl2 O5 109.56(18) . . ? 
O2 Cl2 O5 110.2(2) . . ? 
O3 Cl2 O5 109.33(19) . . ? 
C6 N3 C7 111.6(3) . . ? 
C6 N3 Ni1 115.7(2) . . ? 
C7 N3 Ni1 111.5(2) . . ? 
C4 N2 C3 116.2(3) . . ? 
C4 N2 Ni1 117.2(2) . . ? 
C3 N2 Ni1 106.1(2) . . ? 
C1 N1 C9 121.9(3) . . ? 
C1 N1 Ni1 126.8(3) . . ? 
C9 N1 Ni1 111.2(2) . . ? 
C1 C2 C3 121.8(3) . . ? 
C6 C5 C4 114.5(3) . . ? 
N2 C3 C12 111.1(3) . . ? 
N2 C3 C11 107.0(3) . . ? 
C12 C3 C11 109.3(3) . . ? 
N2 C3 C2 110.7(3) . . ? 
C12 C3 C2 108.0(3) . . ? 
C11 C3 C2 110.8(3) . . ? 
N3 C6 C5 113.1(3) . . ? 
N2 C4 C5 111.3(3) . . ? 
N3 C7 C8 113.6(3) . . ? 
N1 C1 C10 124.0(4) . . ? 
N1 C1 C2 122.0(3) . . ? 
C10 C1 C2 114.1(3) . . ? 
N1 C9 C8 110.6(3) . . ? 
C9 C8 C7 115.8(3) . . ? 

_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full               0.50 
_diffrn_measured_fraction_theta_full   0.000 
_refine_diff_density_max    0.516 
_refine_diff_density_min   -0.820 
_refine_diff_density_rms    0.081 

data_6me1 

_database_code_CSD	182500


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C19 H33 F6 N4 Ni O P' 
_chemical_formula_weight          537.17 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0033   0.0016 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0106   0.0060 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'F'  'F'   0.0171   0.0103 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'P'  'P'   0.1023   0.0942 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Ni'  'Ni'   0.3393   1.1124 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 

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

_cell_length_a                    9.2990(9) 
_cell_length_b                    10.5724(10) 
_cell_length_c                    12.8248(13) 
_cell_angle_alpha                 108.628(7) 
_cell_angle_beta                  95.446(7) 
_cell_angle_gamma                 97.430(6) 
_cell_volume                      1172.2(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     64 
_cell_measurement_theta_min       4.791 
_cell_measurement_theta_max       12.307 

_exptl_crystal_description        lath 
_exptl_crystal_colour             blue 
_exptl_crystal_size_max           0.60 
_exptl_crystal_size_mid           0.40 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.522 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              560 
_exptl_absorpt_coefficient_mu     0.962 
_exptl_absorpt_correction_type    psi-scan 
_exptl_absorpt_correction_T_min   0.742 
_exptl_absorpt_correction_T_max   0.900 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             4263 
_diffrn_reflns_av_R_equivalents   0.0500 
_diffrn_reflns_av_sigmaI/netI     0.0731 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          3.05 
_diffrn_reflns_theta_max          24.99 
_reflns_number_total              4023 
_reflns_number_gt                 2661 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_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^)+(0.1375P)^2^+0.4896P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      Patterson 
_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          4023 
_refine_ls_number_parameters      289 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1162 
_refine_ls_R_factor_gt            0.0740 
_refine_ls_wR_factor_ref          0.2570 
_refine_ls_wR_factor_gt           0.2001 
_refine_ls_goodness_of_fit_ref    1.205 
_refine_ls_restrained_S_all       1.205 
_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 0.71870(10) 0.69468(9) 0.69915(8) 0.0301(3) Uani 1 1 d . . . 
P1 P 0.3510(3) 0.1802(3) 0.8101(2) 0.0582(7) Uani 1 1 d . . . 
O1 O 0.8340(6) 0.5861(6) 0.5838(4) 0.0414(13) Uani 1 1 d . . . 
N4 N 0.8183(7) 0.5424(6) 0.7416(5) 0.0350(15) Uani 1 1 d . . . 
C16 C 0.9882(9) 0.3444(9) 0.6850(7) 0.045(2) Uani 1 1 d . . . 
H16 H 1.0478 0.2761 0.6675 0.054 Uiso 1 1 calc R . . 
C18 C 0.8721(8) 0.5140(8) 0.6448(6) 0.0361(18) Uani 1 1 d . . . 
C15 C 0.9299(9) 0.3739(9) 0.7826(7) 0.044(2) Uani 1 1 d . . . 
H15 H 0.9476 0.3238 0.8308 0.053 Uiso 1 1 calc R . . 
C14 C 0.8458(10) 0.4753(9) 0.8124(8) 0.046(2) Uani 1 1 d . . . 
C17 C 0.9609(9) 0.4130(8) 0.6120(7) 0.043(2) Uani 1 1 d . . . 
H17 H 0.9994 0.3936 0.5436 0.051 Uiso 1 1 calc R . . 
N3 N 0.8706(6) 0.8725(6) 0.7639(5) 0.0326(14) Uani 1 1 d . . . 
N2 N 0.5724(6) 0.7312(6) 0.8071(5) 0.0282(13) Uani 1 1 d . . . 
H2 H 0.5963 0.6892 0.8585 0.034 Uiso 1 1 calc R . . 
N1 N 0.6011(7) 0.7658(6) 0.5963(5) 0.0320(14) Uani 1 1 d . . . 
C3 C 0.4260(8) 0.6536(8) 0.7415(7) 0.0352(17) Uani 1 1 d . . . 
C2 C 0.3679(8) 0.7267(8) 0.6624(7) 0.0369(18) Uani 1 1 d . . . 
H2A H 0.2800 0.6662 0.6136 0.044 Uiso 1 1 calc R . . 
H2B H 0.3343 0.8086 0.7091 0.044 Uiso 1 1 calc R . . 
C1 C 0.4650(9) 0.7701(7) 0.5889(6) 0.0355(18) Uani 1 1 d . . . 
C13 C 1.0013(8) 0.8410(9) 0.8218(7) 0.043(2) Uani 1 1 d . . . 
H13A H 1.0372 0.7657 0.7699 0.064 Uiso 1 1 calc R . . 
H13B H 0.9739 0.8158 0.8853 0.064 Uiso 1 1 calc R . . 
H13C H 1.0787 0.9210 0.8481 0.064 Uiso 1 1 calc R . . 
C12 C 0.4481(10) 0.5119(8) 0.6726(7) 0.043(2) Uani 1 1 d . . . 
H12A H 0.5211 0.5193 0.6235 0.064 Uiso 1 1 calc R . . 
H12B H 0.3550 0.4607 0.6276 0.064 Uiso 1 1 calc R . . 
H12C H 0.4825 0.4649 0.7223 0.064 Uiso 1 1 calc R . . 
C11 C 0.3114(9) 0.6433(9) 0.8191(8) 0.047(2) Uani 1 1 d . . . 
H11A H 0.3469 0.5989 0.8706 0.071 Uiso 1 1 calc R . . 
H11B H 0.2188 0.5902 0.7746 0.071 Uiso 1 1 calc R . . 
H11C H 0.2958 0.7344 0.8615 0.071 Uiso 1 1 calc R . . 
C6 C 0.8163(9) 0.9879(8) 0.8428(7) 0.041(2) Uani 1 1 d . . . 
H6A H 0.7548 1.0286 0.7993 0.050 Uiso 1 1 calc R . . 
H6B H 0.9015 1.0579 0.8850 0.050 Uiso 1 1 calc R . . 
C10 C 0.3826(10) 0.8232(10) 0.5079(8) 0.054(2) Uani 1 1 d . . . 
H10A H 0.4502 0.8505 0.4618 0.081 Uiso 1 1 calc R . . 
H10B H 0.3409 0.9016 0.5495 0.081 Uiso 1 1 calc R . . 
H10C H 0.3035 0.7519 0.4602 0.081 Uiso 1 1 calc R . . 
C5 C 0.7274(9) 0.9485(8) 0.9249(6) 0.0388(19) Uani 1 1 d . . . 
H5A H 0.7216 1.0313 0.9871 0.047 Uiso 1 1 calc R . . 
H5B H 0.7792 0.8895 0.9562 0.047 Uiso 1 1 calc R . . 
C8 C 0.8043(10) 0.9372(9) 0.5917(7) 0.047(2) Uani 1 1 d . . . 
H8A H 0.7513 1.0065 0.6358 0.056 Uiso 1 1 calc R . . 
H8B H 0.8521 0.9747 0.5397 0.056 Uiso 1 1 calc R . . 
C4 C 0.5722(9) 0.8745(8) 0.8727(7) 0.0417(19) Uani 1 1 d . . . 
H4A H 0.5104 0.8787 0.9320 0.050 Uiso 1 1 calc R . . 
H4B H 0.5295 0.9201 0.8237 0.050 Uiso 1 1 calc R . . 
C7 C 0.9250(9) 0.9142(9) 0.6718(7) 0.046(2) Uani 1 1 d . . . 
H7A H 0.9768 0.8435 0.6283 0.055 Uiso 1 1 calc R . . 
H7B H 0.9972 0.9989 0.7048 0.055 Uiso 1 1 calc R . . 
C9 C 0.6940(9) 0.8142(8) 0.5247(6) 0.0399(19) Uani 1 1 d . . . 
H9A H 0.6311 0.8364 0.4685 0.048 Uiso 1 1 calc R . . 
H9B H 0.7458 0.7412 0.4849 0.048 Uiso 1 1 calc R . . 
C19 C 0.7797(12) 0.5134(11) 0.9184(8) 0.063(3) Uani 1 1 d . . . 
H19A H 0.7262 0.5883 0.9219 0.094 Uiso 1 1 calc R . . 
H19B H 0.8577 0.5415 0.9822 0.094 Uiso 1 1 calc R . . 
H19C H 0.7120 0.4352 0.9202 0.094 Uiso 1 1 calc R . . 
F1 F 0.3246(8) 0.0375(7) 0.8204(8) 0.099(3) Uani 1 1 d . . . 
F2 F 0.1949(9) 0.1954(7) 0.8629(6) 0.096(2) Uani 1 1 d . . . 
F3 F 0.2467(8) 0.1271(12) 0.6955(7) 0.130(4) Uani 1 1 d . . . 
F4 F 0.4857(8) 0.1616(12) 0.7533(8) 0.136(4) Uani 1 1 d . . . 
F5 F 0.4353(11) 0.2386(11) 0.9274(7) 0.155(5) Uani 1 1 d . . . 
F6 F 0.3532(14) 0.3199(11) 0.8015(13) 0.183(6) 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 
Ni1 0.0336(6) 0.0294(5) 0.0272(5) 0.0077(4) 0.0025(4) 0.0106(4) 
P1 0.092(2) 0.0479(15) 0.0388(13) 0.0229(11) 0.0029(13) 0.0084(13) 
O1 0.054(3) 0.044(3) 0.036(3) 0.018(3) 0.013(3) 0.024(3) 
N4 0.035(3) 0.038(4) 0.034(3) 0.010(3) 0.011(3) 0.014(3) 
C16 0.040(5) 0.044(5) 0.053(5) 0.014(4) 0.010(4) 0.015(4) 
C18 0.038(4) 0.034(4) 0.030(4) 0.002(3) 0.008(3) 0.007(3) 
C15 0.049(5) 0.043(5) 0.046(5) 0.021(4) 0.000(4) 0.015(4) 
C14 0.047(5) 0.042(5) 0.049(5) 0.016(4) 0.007(4) 0.004(4) 
C17 0.036(4) 0.043(5) 0.045(5) 0.006(4) 0.011(4) 0.011(4) 
N3 0.030(3) 0.033(3) 0.035(3) 0.012(3) -0.004(3) 0.009(3) 
N2 0.037(3) 0.028(3) 0.019(3) 0.006(2) 0.000(2) 0.011(3) 
N1 0.043(4) 0.025(3) 0.022(3) 0.002(2) -0.003(3) 0.006(3) 
C3 0.025(4) 0.031(4) 0.047(5) 0.011(3) 0.001(3) 0.006(3) 
C2 0.032(4) 0.034(4) 0.039(4) 0.008(3) -0.009(3) 0.008(3) 
C1 0.043(5) 0.022(4) 0.036(4) 0.003(3) -0.006(3) 0.009(3) 
C13 0.030(4) 0.053(5) 0.045(5) 0.020(4) -0.011(3) 0.011(4) 
C12 0.051(5) 0.033(4) 0.035(4) 0.003(4) 0.000(4) 0.003(4) 
C11 0.042(5) 0.048(5) 0.049(5) 0.016(4) 0.008(4) 0.002(4) 
C6 0.044(5) 0.033(4) 0.036(4) -0.001(3) 0.001(4) -0.002(4) 
C10 0.054(6) 0.054(6) 0.053(6) 0.022(5) -0.010(4) 0.006(4) 
C5 0.045(5) 0.033(4) 0.028(4) 0.000(3) -0.001(3) 0.005(3) 
C8 0.059(5) 0.040(5) 0.042(5) 0.020(4) -0.002(4) 0.000(4) 
C4 0.038(4) 0.035(4) 0.045(5) 0.006(4) 0.002(4) 0.004(3) 
C7 0.036(4) 0.055(5) 0.047(5) 0.020(4) 0.008(4) -0.003(4) 
C9 0.053(5) 0.041(5) 0.025(4) 0.013(3) -0.003(3) 0.008(4) 
C19 0.089(8) 0.066(7) 0.046(6) 0.028(5) 0.018(5) 0.028(6) 
F1 0.083(5) 0.061(4) 0.164(8) 0.045(5) 0.017(5) 0.029(4) 
F2 0.123(6) 0.078(5) 0.092(5) 0.017(4) 0.059(5) 0.028(4) 
F3 0.077(5) 0.262(13) 0.083(6) 0.098(7) 0.015(4) 0.033(6) 
F4 0.059(4) 0.251(12) 0.127(8) 0.093(8) 0.022(5) 0.043(6) 
F5 0.153(9) 0.203(11) 0.068(5) 0.049(6) -0.042(5) -0.081(8) 
F6 0.205(12) 0.131(9) 0.293(16) 0.157(11) 0.089(11) 0.046(8) 

_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 N1 2.018(6) . ? 
Ni1 N2 2.017(6) . ? 
Ni1 O1 2.047(5) . ? 
Ni1 N3 2.077(6) . ? 
Ni1 N4 2.144(6) . ? 
Ni1 C18 2.492(7) . ? 
P1 F4 1.511(8) . ? 
P1 F6 1.514(9) . ? 
P1 F5 1.522(8) . ? 
P1 F1 1.546(7) . ? 
P1 F3 1.574(8) . ? 
P1 F2 1.664(7) . ? 
O1 C18 1.310(9) . ? 
N4 C18 1.342(10) . ? 
N4 C14 1.345(11) . ? 
C16 C15 1.372(12) . ? 
C16 C17 1.380(12) . ? 
C18 C17 1.417(11) . ? 
C15 C14 1.385(12) . ? 
C14 C19 1.504(13) . ? 
N3 C13 1.493(9) . ? 
N3 C7 1.494(10) . ? 
N3 C6 1.495(10) . ? 
N2 C4 1.479(9) . ? 
N2 C3 1.513(9) . ? 
N1 C1 1.269(10) . ? 
N1 C9 1.478(10) . ? 
C3 C12 1.529(10) . ? 
C3 C11 1.542(11) . ? 
C3 C2 1.557(11) . ? 
C2 C1 1.498(12) . ? 
C1 C10 1.522(11) . ? 
C6 C5 1.524(11) . ? 
C5 C4 1.528(11) . ? 
C8 C9 1.502(11) . ? 
C8 C7 1.545(12) . ? 

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 
N1 Ni1 N2 90.8(2) . . ? 
N1 Ni1 O1 96.9(2) . . ? 
N2 Ni1 O1 158.7(2) . . ? 
N1 Ni1 N3 93.3(2) . . ? 
N2 Ni1 N3 101.0(2) . . ? 
O1 Ni1 N3 98.3(2) . . ? 
N1 Ni1 N4 154.2(2) . . ? 
N2 Ni1 N4 101.5(2) . . ? 
O1 Ni1 N4 64.2(2) . . ? 
N3 Ni1 N4 106.2(2) . . ? 
N1 Ni1 C18 126.8(3) . . ? 
N2 Ni1 C18 132.5(3) . . ? 
O1 Ni1 C18 31.7(2) . . ? 
N3 Ni1 C18 103.9(2) . . ? 
N4 Ni1 C18 32.6(2) . . ? 
F4 P1 F6 91.8(6) . . ? 
F4 P1 F5 95.0(6) . . ? 
F6 P1 F5 91.8(7) . . ? 
F4 P1 F1 96.0(5) . . ? 
F6 P1 F1 171.6(6) . . ? 
F5 P1 F1 90.7(5) . . ? 
F4 P1 F3 92.0(5) . . ? 
F6 P1 F3 86.0(7) . . ? 
F5 P1 F3 172.7(6) . . ? 
F1 P1 F3 90.5(5) . . ? 
F4 P1 F2 175.6(5) . . ? 
F6 P1 F2 88.2(6) . . ? 
F5 P1 F2 89.4(5) . . ? 
F1 P1 F2 83.8(4) . . ? 
F3 P1 F2 83.6(4) . . ? 
C18 O1 Ni1 93.2(4) . . ? 
C18 N4 C14 121.4(7) . . ? 
C18 N4 Ni1 88.1(5) . . ? 
C14 N4 Ni1 150.5(6) . . ? 
C15 C16 C17 120.6(8) . . ? 
O1 C18 N4 114.4(6) . . ? 
O1 C18 C17 123.5(7) . . ? 
N4 C18 C17 122.1(8) . . ? 
O1 C18 Ni1 55.1(3) . . ? 
N4 C18 Ni1 59.3(4) . . ? 
C17 C18 Ni1 178.5(7) . . ? 
C16 C15 C14 121.4(8) . . ? 
N4 C14 C15 118.4(8) . . ? 
N4 C14 C19 117.5(8) . . ? 
C15 C14 C19 124.1(9) . . ? 
C16 C17 C18 116.1(8) . . ? 
C13 N3 C7 105.2(6) . . ? 
C13 N3 C6 109.5(6) . . ? 
C7 N3 C6 109.6(6) . . ? 
C13 N3 Ni1 107.3(5) . . ? 
C7 N3 Ni1 110.2(5) . . ? 
C6 N3 Ni1 114.6(5) . . ? 
C4 N2 C3 115.0(6) . . ? 
C4 N2 Ni1 117.0(5) . . ? 
C3 N2 Ni1 105.8(4) . . ? 
C1 N1 C9 121.4(7) . . ? 
C1 N1 Ni1 127.2(6) . . ? 
C9 N1 Ni1 111.4(5) . . ? 
N2 C3 C12 108.1(6) . . ? 
N2 C3 C11 111.3(7) . . ? 
C12 C3 C11 110.0(7) . . ? 
N2 C3 C2 109.9(6) . . ? 
C12 C3 C2 109.4(7) . . ? 
C11 C3 C2 108.3(6) . . ? 
C1 C2 C3 120.6(6) . . ? 
N1 C1 C2 123.2(7) . . ? 
N1 C1 C10 124.4(8) . . ? 
C2 C1 C10 112.4(7) . . ? 
N3 C6 C5 114.2(7) . . ? 
C6 C5 C4 113.2(7) . . ? 
C9 C8 C7 115.8(7) . . ? 
N2 C4 C5 111.1(6) . . ? 
N3 C7 C8 114.6(7) . . ? 
N1 C9 C8 111.4(6) . . ? 

_diffrn_measured_fraction_theta_max    0.978 
_diffrn_reflns_theta_full               0.50 
_diffrn_measured_fraction_theta_full   0.000 
_refine_diff_density_max    1.190 
_refine_diff_density_min   -0.985 
_refine_diff_density_rms    0.149