# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         1350

loop_
_publ_author_name
'Song Gao'
'Ru-Yin Li'
'Zhe-Ming Wang'

_publ_contact_author_name        'Song Gao'
_publ_contact_author_email       GAOSONG@PKU.EDU.CN

_publ_section_title              
;
M2(N3)4(hmt)(H2O) (M = Co2+ and Ni2+, hmt =
hexamethylenetetramine): Mixed Azide-hmt Bridged 3D Metal Frameworks
with Long-Range Magnetic Ordering
;

# Attachment 'GAOS-20090402-cif.CIF'

data_last
_database_code_depnum_ccdc_archive 'CCDC 725954'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H14 Co2 N16 O'
_chemical_formula_weight         444.19

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'

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

_cell_length_a                   11.7392(6)
_cell_length_b                   12.7081(6)
_cell_length_c                   9.5192(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.153(3)
_cell_angle_gamma                90.00
_cell_volume                     1420.10(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13213
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      27.485

_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    2.378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_process_details   'Sortav (Blessing 1995)'

_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  'NONIUS KappaCCD Diffractometer'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9066
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.47
_diffrn_reflns_theta_max         27.50
_reflns_number_total             1707
_reflns_number_gt                1308
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0389P)²+0.0000P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.0020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1707
_refine_ls_number_parameters     131
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0704
_refine_ls_wR_factor_gt          0.0666
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_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
Co1 Co 0.2500 0.2500 0.5000 0.02505(16) Uani 1 2 d S . .
Co2 Co 0.36722(3) 0.0000 0.94503(4) 0.02323(15) Uani 1 2 d S . .
N1 N 0.08892(17) 0.31726(15) 0.4400(2) 0.0298(5) Uani 1 1 d . . .
N2 N 0.0000 0.31473(19) 0.5000 0.0282(6) Uani 1 2 d S . .
N3 N 0.17221(16) 0.17220(15) 0.66337(18) 0.0286(5) Uani 1 1 d . . .
N4 N 0.21828(15) 0.14796(14) 0.76864(19) 0.0265(4) Uani 1 1 d . . .
N5 N 0.26211(18) 0.12629(16) 0.8751(2) 0.0364(5) Uani 1 1 d . . .
N6 N 0.5000 0.1029(2) 1.0000 0.0290(6) Uani 1 2 d S . .
N7 N 0.5000 0.1969(2) 1.0000 0.0334(7) Uani 1 2 d S . .
N8 N 0.5000 0.2856(3) 1.0000 0.0770(14) Uani 1 2 d S . .
N9 N 0.28083(14) 0.40254(13) 0.64277(17) 0.0223(4) Uani 1 1 d . . .
N10 N 0.4298(2) 0.5000 0.7679(3) 0.0260(6) Uani 1 2 d S . .
N11 N 0.2350(2) 0.5000 0.8592(2) 0.0205(5) Uani 1 2 d S . .
C1 C 0.40341(18) 0.40635(18) 0.6857(2) 0.0265(5) Uani 1 1 d . . .
H11 H 0.4214 0.3443 0.7407 0.032 Uiso 1 1 calc R . .
H12 H 0.4507 0.4054 0.6023 0.032 Uiso 1 1 calc R . .
C2 C 0.21149(18) 0.40502(16) 0.7732(2) 0.0220(5) Uani 1 1 d . . .
H21 H 0.1313 0.4036 0.7484 0.026 Uiso 1 1 calc R . .
H22 H 0.2278 0.3427 0.8286 0.026 Uiso 1 1 calc R . .
C3 C 0.2559(3) 0.5000 0.5627(3) 0.0240(7) Uani 1 2 d S . .
H31 H 0.3007 0.5000 0.4772 0.029 Uiso 1 2 calc SR . .
H32 H 0.1761 0.5000 0.5359 0.029 Uiso 1 2 calc SR . .
C4 C 0.3604(2) 0.5000 0.8957(3) 0.0230(7) Uani 1 2 d S . .
H41 H 0.3782 0.5618 0.9514 0.028 Uiso 0.50 1 calc PR . .
H42 H 0.3782 0.4382 0.9514 0.028 Uiso 0.50 1 calc PR . .
O1 O 0.4345(2) 0.0000 0.7314(2) 0.0376(6) Uani 1 2 d S . .
H1 H 0.415(2) 0.069(2) 0.666(3) 0.061(8) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N3 2.0585(18) 7_556 ?
Co1 N3 2.0585(18) . ?
Co1 N1 2.1510(19) 7_556 ?
Co1 N1 2.1510(19) . ?
Co1 N9 2.3944(17) 7_556 ?
Co1 N9 2.3944(17) . ?
Co2 N6 2.1001(16) . ?
Co2 N6 2.1001(16) 5_657 ?
Co2 N5 2.130(2) 6 ?
Co2 N5 2.1301(19) . ?
Co2 O1 2.184(2) . ?
Co2 N11 2.219(2) 7_557 ?
N1 N2 1.192(2) . ?
N2 N1 1.192(2) 2_556 ?
N3 N4 1.178(2) . ?
N4 N5 1.168(3) . ?
N6 N7 1.194(4) . ?
N6 Co2 2.1001(16) 5_657 ?
N7 N8 1.128(4) . ?
N9 C3 1.483(2) . ?
N9 C2 1.487(3) . ?
N9 C1 1.496(3) . ?
N10 C1 1.457(3) . ?
N10 C1 1.457(3) 6_565 ?
N10 C4 1.465(4) . ?
N11 C2 1.484(2) . ?
N11 C2 1.484(2) 6_565 ?
N11 C4 1.512(4) . ?
N11 Co2 2.219(2) 7_557 ?
C1 H11 0.9700 . ?
C1 H12 0.9700 . ?
C2 H21 0.9700 . ?
C2 H22 0.9700 . ?
C3 N9 1.483(2) 6_565 ?
C3 H31 0.9700 . ?
C3 H32 0.9700 . ?
C4 H41 0.9700 . ?
C4 H42 0.9700 . ?
O1 H1 1.10(3) . ?

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
N3 Co1 N3 180.00(9) 7_556 . ?
N3 Co1 N1 90.00(7) 7_556 7_556 ?
N3 Co1 N1 90.00(7) . 7_556 ?
N3 Co1 N1 90.00(7) 7_556 . ?
N3 Co1 N1 90.00(7) . . ?
N1 Co1 N1 180.00(10) 7_556 . ?
N3 Co1 N9 91.53(7) 7_556 7_556 ?
N3 Co1 N9 88.47(7) . 7_556 ?
N1 Co1 N9 87.73(6) 7_556 7_556 ?
N1 Co1 N9 92.27(6) . 7_556 ?
N3 Co1 N9 88.47(7) 7_556 . ?
N3 Co1 N9 91.53(7) . . ?
N1 Co1 N9 92.27(6) 7_556 . ?
N1 Co1 N9 87.73(6) . . ?
N9 Co1 N9 180.0 7_556 . ?
N6 Co2 N6 77.06(11) . 5_657 ?
N6 Co2 N5 167.47(7) . 6 ?
N6 Co2 N5 92.15(8) 5_657 6 ?
N6 Co2 N5 92.15(8) . . ?
N6 Co2 N5 167.47(8) 5_657 . ?
N5 Co2 N5 97.78(12) 6 . ?
N6 Co2 O1 87.82(5) . . ?
N6 Co2 O1 87.82(5) 5_657 . ?
N5 Co2 O1 85.39(7) 6 . ?
N5 Co2 O1 85.39(7) . . ?
N6 Co2 N11 101.15(5) . 7_557 ?
N6 Co2 N11 101.15(5) 5_657 7_557 ?
N5 Co2 N11 87.04(7) 6 7_557 ?
N5 Co2 N11 87.04(7) . 7_557 ?
O1 Co2 N11 168.48(9) . 7_557 ?
N2 N1 Co1 129.24(15) . . ?
N1 N2 N1 176.9(3) . 2_556 ?
N4 N3 Co1 124.37(15) . . ?
N5 N4 N3 177.9(2) . . ?
N4 N5 Co2 134.60(17) . . ?
N7 N6 Co2 128.53(5) . . ?
N7 N6 Co2 128.53(5) . 5_657 ?
Co2 N6 Co2 102.94(11) . 5_657 ?
N8 N7 N6 180.000(1) . . ?
C3 N9 C2 107.69(18) . . ?
C3 N9 C1 107.57(18) . . ?
C2 N9 C1 107.43(15) . . ?
C3 N9 Co1 110.79(12) . . ?
C2 N9 Co1 114.13(12) . . ?
C1 N9 Co1 108.98(12) . . ?
C1 N10 C1 109.5(2) . 6_565 ?
C1 N10 C4 109.16(16) . . ?
C1 N10 C4 109.16(16) 6_565 . ?
C2 N11 C2 108.9(2) . 6_565 ?
C2 N11 C4 107.85(15) . . ?
C2 N11 C4 107.85(15) 6_565 . ?
C2 N11 Co2 111.27(13) . 7_557 ?
C2 N11 Co2 111.27(13) 6_565 7_557 ?
C4 N11 Co2 109.58(17) . 7_557 ?
N10 C1 N9 112.08(18) . . ?
N10 C1 H11 109.2 . . ?
N9 C1 H11 109.2 . . ?
N10 C1 H12 109.2 . . ?
N9 C1 H12 109.2 . . ?
H11 C1 H12 107.9 . . ?
N11 C2 N9 112.10(17) . . ?
N11 C2 H21 109.2 . . ?
N9 C2 H21 109.2 . . ?
N11 C2 H22 109.2 . . ?
N9 C2 H22 109.2 . . ?
H21 C2 H22 107.9 . . ?
N9 C3 N9 113.2(2) 6_565 . ?
N9 C3 H31 108.9 6_565 . ?
N9 C3 H31 108.9 . . ?
N9 C3 H32 108.9 6_565 . ?
N9 C3 H32 108.9 . . ?
H31 C3 H32 107.7 . . ?
N10 C4 N11 110.6(2) . . ?
N10 C4 H41 109.5 . . ?
N11 C4 H41 109.5 . . ?
N10 C4 H42 109.5 . . ?
N11 C4 H42 109.5 . . ?
H41 C4 H42 108.1 . . ?
Co2 O1 H1 116.8(15) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.150



