Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2001

data_ind35
_database_code_CSD            155222
_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Chaudhuri, Nirmalendu Ray'
'Dalai, Sudipta'
'Lloret, F.'
'Mukherjee, Partha Sarathi'
'Zangrando, Ennio'

_publ_contact_author_name     	'Prof Nirmalendu Ray Chaudhuri'  
_publ_contact_author_address 
;
Prof Nirmalendu Ray Chaudhuri
Department of Chemistry
Indian Association for the Cultivation of Science
Jadavpur
Calcutta
700 032
INDIA
;

_publ_contact_author_email       'ICNRC@MAHENDRA.IACS.RES.IN'

_publ_section_title
;
The first metamagnetic one-dimensional molecular material with
nickel(II) and end-to-end azido bridge
;

_audit_creation_method            SHELXL
_chemical_name_systematic
;
catena-(mu-azido)(azido)(N-2-pyridinmethylene-
(N’,N’,2,2-tetramethyl-propandiamine))nickel(II)
;
_chemical_name_common             ?
_chemical_formula_moiety          '(N3 1-)2, (C13 H21 N3), (Ni 2+)'
_chemical_formula_structural      'catena-((N3)2 (C13 H21 N3)Ni)'
_chemical_formula_analytical      ?
_chemical_formula_sum             'C13 H21 N9 Ni'
_chemical_formula_weight          362.10
_chemical_melting_point           ?
_chemical_compound_source         ?

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'
'Ni'  'Ni'   0.3393   1.1124
'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'

_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    'P 21/n'

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

_cell_length_a                    11.922(3)
_cell_length_b                    8.360(2)
_cell_length_c                    17.121(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  101.42(2)
_cell_angle_gamma                 90.00
_cell_volume                      1672.6(8)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     25
_cell_measurement_theta_min       10
_cell_measurement_theta_max       15

_exptl_crystal_description        'prism'
_exptl_crystal_colour             'deep green'
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.438
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              760
_exptl_absorpt_coefficient_mu     1.174
_exptl_absorpt_correction_type    psi-scan
_exptl_absorpt_correction_T_min      0.8838
_exptl_absorpt_correction_T_max      0.9998

_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_detector                 'scintillation LiI'
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method        'non-profiled omega scans'
_diffrn_standards_number          3
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   333
_diffrn_standards_decay_%         2
_diffrn_reflns_number             4025
_diffrn_reflns_av_R_equivalents   0.0548
_diffrn_reflns_av_sigmaI/netI     0.1763
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          2.31
_diffrn_reflns_theta_max          27.98
_reflns_number_total              3295
_reflns_number_observed           1628
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        'CAD4 (Enraf-Nonius)'
_computing_cell_refinement        'CELDIM (Enraf-Nonius)'
_computing_data_reduction         'WinGX 1.63 (Farrugia, 1999)'
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Ortep3/Windows (Farrugia,1997)'
_computing_publication_material   'WinGX 1.63 (Farrugia, 1999)' 


_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 730 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0622P)^2^] 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     ?
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          3295
_refine_ls_number_parameters      212
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.2108
_refine_ls_R_factor_obs           0.0611
_refine_ls_wR_factor_all          0.1607
_refine_ls_wR_factor_obs          0.1184
_refine_ls_goodness_of_fit_all    0.947
_refine_ls_goodness_of_fit_obs    1.122
_refine_ls_restrained_S_all       0.939
_refine_ls_restrained_S_obs       1.122
_refine_ls_shift/esd_max          0.004
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni Ni 0.41287(6) 0.12353(10) 0.26324(4) 0.0345(2) Uani 1 d . .
N1 N 0.3690(4) 0.1149(8) 0.3776(3) 0.0422(13) Uani 1 d . .
N2 N 0.4426(4) -0.1099(6) 0.2928(3) 0.0368(11) Uani 1 d . .
N3 N 0.4650(4) 0.1014(6) 0.1487(3) 0.0377(12) Uani 1 d . .
N4 N 0.5726(4) 0.2003(7) 0.3221(3) 0.0496(15) Uani 1 d . .
N5 N 0.5897(5) 0.3241(8) 0.3544(3) 0.054(2) Uani 1 d . .
N6 N 0.6090(7) 0.4452(10) 0.3873(5) 0.111(3) Uani 1 d . .
N7 N 0.3639(4) 0.3602(7) 0.2354(3) 0.0445(13) Uani 1 d . .
N8 N 0.3087(4) 0.4515(6) 0.2623(3) 0.0358(12) Uani 1 d . .
N9 N 0.2441(4) 0.0489(6) 0.2104(3) 0.0414(13) Uani 1 d . .
C1 C 0.3391(6) 0.2319(10) 0.4217(4) 0.057(2) Uani 1 d . .
H1 H 0.3329(6) 0.3354(10) 0.4014(4) 0.068 Uiso 1 calc R .
C2 C 0.3165(6) 0.2047(12) 0.4978(4) 0.066(2) Uani 1 d . .
H2 H 0.2966(6) 0.2890(12) 0.5277(4) 0.079 Uiso 1 calc R .
C3 C 0.3241(6) 0.0529(11) 0.5273(4) 0.061(2) Uani 1 d . .
H3 H 0.3068(6) 0.0315(11) 0.5768(4) 0.074 Uiso 1 calc R .
C4 C 0.3575(5) -0.0670(9) 0.4831(4) 0.048(2) Uani 1 d . .
H4 H 0.3651(5) -0.1712(9) 0.5025(4) 0.057 Uiso 1 calc R .
C5 C 0.3799(5) -0.0310(8) 0.4088(4) 0.040(2) Uani 1 d . .
C6 C 0.4175(5) -0.1534(8) 0.3587(4) 0.044(2) Uani 1 d . .
H6 H 0.4230(5) -0.2601(8) 0.3744(4) 0.053 Uiso 1 calc R .
C7 C 0.4698(6) -0.2364(8) 0.2401(4) 0.048(2) Uani 1 d . .
H7A H 0.3991(6) -0.2749(8) 0.2074(4) 0.058 Uiso 1 calc R .
H7B H 0.5048(6) -0.3251(8) 0.2725(4) 0.058 Uiso 1 calc R .
C8 C 0.5493(6) -0.1834(8) 0.1862(4) 0.047(2) Uani 1 d . .
C9 C 0.4894(6) -0.0639(8) 0.1254(4) 0.050(2) Uani 1 d . .
H9A H 0.5347(6) -0.0552(8) 0.0844(4) 0.060 Uiso 1 calc R .
H9B H 0.4168(6) -0.1111(8) 0.1005(4) 0.060 Uiso 1 calc R .
C10 C 0.5736(8) -0.3319(9) 0.1399(5) 0.082(3) Uani 1 d . .
H10A H 0.5034(10) -0.3700(38) 0.1078(25) 0.122 Uiso 1 calc R .
H10B H 0.6063(43) -0.4139(25) 0.1767(5) 0.122 Uiso 1 calc R .
H10C H 0.6262(36) -0.3048(18) 0.1062(24) 0.122 Uiso 1 calc R .
C11 C 0.6619(5) -0.1257(10) 0.2369(4) 0.070(2) Uani 1 d . .
H11A H 0.6478(8) -0.0344(38) 0.2676(23) 0.105 Uiso 1 calc R .
H11B H 0.7136(17) -0.0965(59) 0.2028(5) 0.105 Uiso 1 calc R .
H11C H 0.6952(22) -0.2098(22) 0.2721(22) 0.105 Uiso 1 calc R .
C12 C 0.3693(5) 0.1627(8) 0.0857(3) 0.051(2) Uani 1 d . .
H12A H 0.3016(11) 0.1008(32) 0.0860(17) 0.077 Uiso 1 calc R .
H12B H 0.3902(15) 0.1539(47) 0.0345(4) 0.077 Uiso 1 calc R .
H12C H 0.3548(23) 0.2728(16) 0.0962(14) 0.077 Uiso 1 calc R .
C13 C 0.5634(6) 0.2063(9) 0.1469(4) 0.060(2) Uani 1 d . .
H13A H 0.5465(15) 0.3124(14) 0.1627(25) 0.090 Uiso 1 calc R .
H13B H 0.5785(24) 0.2090(42) 0.0939(7) 0.090 Uiso 1 calc R .
H13C H 0.6294(10) 0.1661(30) 0.1830(20) 0.090 Uiso 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
Ni 0.0310(4) 0.0376(4) 0.0358(4) 0.0024(5) 0.0084(3) 0.0012(5)
N1 0.036(3) 0.053(4) 0.038(3) -0.001(3) 0.007(2) -0.004(3)
N2 0.031(2) 0.038(3) 0.041(3) 0.003(3) 0.008(2) 0.002(3)
N3 0.037(3) 0.039(3) 0.041(3) 0.003(3) 0.014(2) 0.002(3)
N4 0.038(3) 0.054(4) 0.055(4) -0.012(3) 0.003(3) -0.003(3)
N5 0.044(3) 0.071(5) 0.048(4) -0.004(3) 0.010(3) -0.010(3)
N6 0.120(7) 0.078(6) 0.130(7) -0.052(5) 0.016(5) -0.024(5)
N7 0.041(3) 0.045(4) 0.052(3) 0.000(3) 0.020(2) 0.006(3)
N8 0.024(3) 0.042(3) 0.040(3) 0.002(3) 0.003(2) -0.006(2)
N9 0.034(3) 0.047(3) 0.043(3) 0.005(3) 0.007(2) -0.003(3)
C1 0.051(4) 0.070(5) 0.045(4) 0.003(4) -0.002(3) 0.012(4)
C2 0.058(5) 0.103(7) 0.036(4) -0.012(5) 0.009(4) 0.006(5)
C3 0.054(5) 0.091(6) 0.038(4) 0.005(5) 0.007(4) -0.005(4)
C4 0.045(4) 0.060(5) 0.034(4) 0.011(3) -0.004(3) -0.012(3)
C5 0.036(4) 0.038(4) 0.042(4) 0.004(3) 0.000(3) -0.004(3)
C6 0.041(3) 0.037(4) 0.052(4) 0.006(3) 0.001(3) -0.014(3)
C7 0.050(4) 0.043(4) 0.053(4) 0.003(3) 0.011(3) 0.007(3)
C8 0.050(4) 0.042(4) 0.052(4) -0.002(3) 0.018(3) 0.011(3)
C9 0.064(5) 0.048(4) 0.044(4) 0.006(3) 0.022(4) 0.006(4)
C10 0.118(7) 0.049(6) 0.088(6) -0.004(4) 0.046(6) 0.017(5)
C11 0.043(4) 0.077(5) 0.090(5) 0.018(5) 0.016(4) 0.018(5)
C12 0.046(4) 0.067(6) 0.042(3) 0.007(3) 0.011(3) 0.013(4)
C13 0.058(5) 0.062(5) 0.069(5) 0.000(4) 0.036(4) -0.016(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.
;

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
Ni N2 2.030(5) . ?
Ni N4 2.072(5) . ?
Ni N7 2.091(6) . ?
Ni N1 2.125(5) . ?
Ni N9 2.130(5) . ?
Ni N3 2.180(5) . ?
N1 C1 1.327(8) . ?
N1 C5 1.327(8) . ?
N2 C6 1.275(7) . ?
N2 C7 1.467(8) . ?
N3 C13 1.469(7) . ?
N3 C9 1.483(8) . ?
N3 C12 1.497(7) . ?
N4 N5 1.172(8) . ?
N5 N6 1.159(8) . ?
N7 N8 1.161(6) . ?
N8 N9 1.180(6) 2 ?
N9 N8 1.180(6) 2_545 ?
C1 C2 1.400(9) . ?
C2 C3 1.362(11) . ?
C3 C4 1.362(9) . ?
C4 C5 1.384(8) . ?
C5 C6 1.462(9) . ?
C7 C8 1.515(9) . ?
C8 C9 1.515(9) . ?
C8 C11 1.526(9) . ?
C8 C10 1.531(9) . ?

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 Ni N4 94.5(2) . . ?
N2 Ni N7 173.6(2) . . ?
N4 Ni N7 90.4(2) . . ?
N2 Ni N1 78.5(2) . . ?
N4 Ni N1 86.1(2) . . ?
N7 Ni N1 97.7(2) . . ?
N2 Ni N9 85.9(2) . . ?
N4 Ni N9 175.8(2) . . ?
N7 Ni N9 89.0(2) . . ?
N1 Ni N9 89.8(2) . . ?
N2 Ni N3 94.3(2) . . ?
N4 Ni N3 93.8(2) . . ?
N7 Ni N3 89.5(2) . . ?
N1 Ni N3 172.8(2) . . ?
N9 Ni N3 90.4(2) . . ?
C1 N1 C5 117.7(6) . . ?
C1 N1 Ni 129.9(5) . . ?
C5 N1 Ni 112.3(4) . . ?
C6 N2 C7 117.2(6) . . ?
C6 N2 Ni 115.8(4) . . ?
C7 N2 Ni 126.1(4) . . ?
C13 N3 C9 110.6(5) . . ?
C13 N3 C12 106.1(5) . . ?
C9 N3 C12 106.7(5) . . ?
C13 N3 Ni 109.8(4) . . ?
C9 N3 Ni 115.3(4) . . ?
C12 N3 Ni 107.9(3) . . ?
N5 N4 Ni 124.0(5) . . ?
N6 N5 N4 178.3(8) . . ?
N8 N7 Ni 133.3(4) . . ?
N7 N8 N9 177.3(6) . 2 ?
N8 N9 Ni 124.5(4) 2_545 . ?
N1 C1 C2 122.2(7) . . ?
C3 C2 C1 119.1(7) . . ?
C4 C3 C2 119.0(7) . . ?
C3 C4 C5 118.7(7) . . ?
N1 C5 C4 123.3(6) . . ?
N1 C5 C6 115.1(6) . . ?
C4 C5 C6 121.6(6) . . ?
N2 C6 C5 118.2(6) . . ?
N2 C7 C8 113.9(5) . . ?
C9 C8 C7 110.2(5) . . ?
C9 C8 C11 115.1(6) . . ?
C7 C8 C11 109.4(5) . . ?
C9 C8 C10 106.9(5) . . ?
C7 C8 C10 106.5(6) . . ?
C11 C8 C10 108.4(6) . . ?
N3 C9 C8 121.3(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ni N1 C1 175.0(5) . . . . ?
N4 Ni N1 C1 79.7(5) . . . . ?
N7 Ni N1 C1 -10.2(5) . . . . ?
N9 Ni N1 C1 -99.1(5) . . . . ?
N3 Ni N1 C1 169.1(13) . . . . ?
N2 Ni N1 C5 -1.3(4) . . . . ?
N4 Ni N1 C5 -96.6(4) . . . . ?
N7 Ni N1 C5 173.5(4) . . . . ?
N9 Ni N1 C5 84.5(4) . . . . ?
N3 Ni N1 C5 -7.2(17) . . . . ?
N4 Ni N2 C6 88.6(4) . . . . ?
N7 Ni N2 C6 -50.2(19) . . . . ?
N1 Ni N2 C6 3.5(4) . . . . ?
N9 Ni N2 C6 -87.2(4) . . . . ?
N3 Ni N2 C6 -177.3(4) . . . . ?
N4 Ni N2 C7 -103.1(5) . . . . ?
N7 Ni N2 C7 118.1(17) . . . . ?
N1 Ni N2 C7 171.8(5) . . . . ?
N9 Ni N2 C7 81.1(5) . . . . ?
N3 Ni N2 C7 -9.0(5) . . . . ?
N2 Ni N3 C13 -118.9(4) . . . . ?
N4 Ni N3 C13 -24.1(5) . . . . ?
N7 Ni N3 C13 66.2(4) . . . . ?
N1 Ni N3 C13 -113.0(15) . . . . ?
N9 Ni N3 C13 155.2(4) . . . . ?
N2 Ni N3 C9 6.8(4) . . . . ?
N4 Ni N3 C9 101.6(4) . . . . ?
N7 Ni N3 C9 -168.1(4) . . . . ?
N1 Ni N3 C9 12.7(17) . . . . ?
N9 Ni N3 C9 -79.1(4) . . . . ?
N2 Ni N3 C12 125.9(4) . . . . ?
N4 Ni N3 C12 -139.3(4) . . . . ?
N7 Ni N3 C12 -49.0(4) . . . . ?
N1 Ni N3 C12 131.8(14) . . . . ?
N9 Ni N3 C12 40.0(4) . . . . ?
N2 Ni N4 N5 -145.7(6) . . . . ?
N7 Ni N4 N5 30.1(6) . . . . ?
N1 Ni N4 N5 -67.6(6) . . . . ?
N9 Ni N4 N5 -51.1(34) . . . . ?
N3 Ni N4 N5 119.7(6) . . . . ?
Ni N4 N5 N6 164.8(279) . . . . ?
N2 Ni N7 N8 38.0(21) . . . . ?
N4 Ni N7 N8 -100.9(6) . . . . ?
N1 Ni N7 N8 -14.7(6) . . . . ?
N9 Ni N7 N8 75.0(6) . . . . ?
N3 Ni N7 N8 165.4(6) . . . . ?
Ni N7 N8 N9 134.5(125) . . . 2 ?
N2 Ni N9 N8 38.8(5) . . . 2_545 ?
N4 Ni N9 N8 -56.1(33) . . . 2_545 ?
N7 Ni N9 N8 -137.4(5) . . . 2_545 ?
N1 Ni N9 N8 -39.7(5) . . . 2_545 ?
N3 Ni N9 N8 133.1(5) . . . 2_545 ?
C5 N1 C1 C2 -1.6(9) . . . . ?
Ni N1 C1 C2 -177.8(5) . . . . ?
N1 C1 C2 C3 -0.8(11) . . . . ?
C1 C2 C3 C4 2.4(11) . . . . ?
C2 C3 C4 C5 -1.6(11) . . . . ?
C1 N1 C5 C4 2.5(9) . . . . ?
Ni N1 C5 C4 179.3(4) . . . . ?
C1 N1 C5 C6 -177.6(5) . . . . ?
Ni N1 C5 C6 -0.8(6) . . . . ?
C3 C4 C5 N1 -0.9(9) . . . . ?
C3 C4 C5 C6 179.2(6) . . . . ?
C7 N2 C6 C5 -174.4(5) . . . . ?
Ni N2 C6 C5 -5.1(7) . . . . ?
N1 C5 C6 N2 3.9(8) . . . . ?
C4 C5 C6 N2 -176.2(5) . . . . ?
C6 N2 C7 C8 -152.6(5) . . . . ?
Ni N2 C7 C8 39.3(7) . . . . ?
N2 C7 C8 C9 -67.8(7) . . . . ?
N2 C7 C8 C11 59.7(7) . . . . ?
N2 C7 C8 C10 176.6(6) . . . . ?
C13 N3 C9 C8 86.8(7) . . . . ?
C12 N3 C9 C8 -158.2(6) . . . . ?
Ni N3 C9 C8 -38.5(7) . . . . ?
C7 C8 C9 N3 71.8(8) . . . . ?
C11 C8 C9 N3 -52.4(8) . . . . ?
C10 C8 C9 N3 -172.9(6) . . . . ?

_refine_diff_density_max    0.913
_refine_diff_density_min   -0.361
_refine_diff_density_rms    0.086