# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Jiannian Yao.'
'Hongbing Fu.'
'Jin Shi Ma.'
"Al'bina I. Mikhaleva"
'Boris A Trofimov'
'Hao Wang.'
'Yi Zeng.'

_publ_contact_author_name        'Jiannian Yao'
_publ_contact_author_email       JNYAO@ICCAS.AC.CN

_publ_section_title              
;
Facile synthesis of size-tunable
micro-octahedrons via metal-organic coordination
;

# Attachment 'Zn(PyrPy)2.cif'

data_sa18
_database_code_depnum_ccdc_archive 'CCDC 730760'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H14 N4 Zn'
_chemical_formula_sum            'C18 H14 N4 Zn'
_chemical_formula_weight         351.70

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   P4(1)2(1)2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   8.2425(12)
_cell_length_b                   8.2425(12)
_cell_length_c                   23.659(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1607.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    256
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      29.85

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.36
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_exptl_absorpt_coefficient_mu    1.532
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5268
_exptl_absorpt_correction_T_max  0.6086
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12088
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1848
_reflns_number_gt                1829
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.5463P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(18)
_refine_ls_number_reflns         1848
_refine_ls_number_parameters     105
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0780
_refine_ls_wR_factor_gt          0.0778
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.161
_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
Zn1 Zn 0.05814(3) 0.05814(3) 1.0000 0.02888(12) Uani 1 2 d S . .
N1 N 0.2730(2) -0.0405(2) 0.99581(7) 0.0285(4) Uani 1 1 d . . .
N2 N 0.0282(2) -0.0893(2) 1.06869(8) 0.0271(4) Uani 1 1 d . . .
C1 C 0.4136(3) -0.0328(3) 0.96624(10) 0.0345(5) Uani 1 1 d . . .
H1A H 0.4322 0.0359 0.9347 0.041 Uiso 1 1 calc R . .
C2 C 0.5263(3) -0.1394(3) 0.98858(11) 0.0386(6) Uani 1 1 d . . .
H2A H 0.6336 -0.1570 0.9753 0.046 Uiso 1 1 calc R . .
C3 C 0.4519(3) -0.2162(3) 1.03428(10) 0.0361(5) Uani 1 1 d . . .
H3A H 0.4988 -0.2959 1.0583 0.043 Uiso 1 1 calc R . .
C4 C 0.2955(3) -0.1529(3) 1.03790(9) 0.0288(4) Uani 1 1 d . . .
C5 C 0.1641(3) -0.1792(3) 1.07771(8) 0.0273(4) Uani 1 1 d . . .
C6 C 0.1712(3) -0.2855(3) 1.12355(9) 0.0350(5) Uani 1 1 d . . .
H6A H 0.2657 -0.3490 1.1299 0.042 Uiso 1 1 calc R . .
C7 C 0.0404(3) -0.2980(3) 1.15954(10) 0.0407(6) Uani 1 1 d . . .
H7A H 0.0442 -0.3705 1.1907 0.049 Uiso 1 1 calc R . .
C8 C -0.0967(3) -0.2047(3) 1.15018(10) 0.0373(5) Uani 1 1 d . . .
H8A H -0.1874 -0.2114 1.1748 0.045 Uiso 1 1 calc R . .
C9 C -0.0984(3) -0.1018(3) 1.10421(10) 0.0326(5) Uani 1 1 d . . .
H9A H -0.1922 -0.0377 1.0974 0.039 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
Zn1 0.02926(14) 0.02926(14) 0.02812(17) 0.00313(11) -0.00313(11) 0.00194(14)
N1 0.0285(9) 0.0298(9) 0.0271(8) -0.0001(8) -0.0004(7) -0.0011(7)
N2 0.0271(9) 0.0282(9) 0.0259(8) 0.0013(7) -0.0004(7) -0.0003(7)
C1 0.0338(12) 0.0368(13) 0.0328(11) -0.0041(9) 0.0060(9) -0.0044(10)
C2 0.0289(12) 0.0422(13) 0.0446(14) -0.0058(11) 0.0055(9) 0.0012(10)
C3 0.0299(12) 0.0362(12) 0.0421(12) -0.0002(10) -0.0019(10) 0.0046(10)
C4 0.0288(11) 0.0280(11) 0.0295(10) -0.0011(8) -0.0016(9) -0.0012(9)
C5 0.0272(11) 0.0267(11) 0.0282(9) -0.0025(9) -0.0039(8) 0.0007(8)
C6 0.0360(12) 0.0333(11) 0.0356(12) 0.0052(10) -0.0022(10) 0.0059(9)
C7 0.0482(15) 0.0413(13) 0.0326(11) 0.0078(10) 0.0046(11) 0.0023(12)
C8 0.0379(13) 0.0382(13) 0.0357(12) 0.0027(10) 0.0099(10) 0.0012(10)
C9 0.0300(12) 0.0326(12) 0.0352(10) 0.0008(9) 0.0030(9) 0.0012(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
Zn1 N1 1.9513(18) . ?
Zn1 N1 1.9513(18) 7_557 ?
Zn1 N2 2.0444(18) 7_557 ?
Zn1 N2 2.0444(18) . ?
N1 C1 1.355(3) . ?
N1 C4 1.373(3) . ?
N2 C9 1.344(3) . ?
N2 C5 1.360(3) . ?
C1 C2 1.384(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.394(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.393(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.452(3) . ?
C5 C6 1.396(3) . ?
C6 C7 1.378(3) . ?
C6 H6A 0.9500 . ?
C7 C8 1.385(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.379(3) . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9500 . ?

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 Zn1 N1 139.35(11) . 7_557 ?
N1 Zn1 N2 116.68(7) . 7_557 ?
N1 Zn1 N2 84.40(7) 7_557 7_557 ?
N1 Zn1 N2 84.40(7) . . ?
N1 Zn1 N2 116.68(7) 7_557 . ?
N2 Zn1 N2 119.22(10) 7_557 . ?
C1 N1 C4 106.88(18) . . ?
C1 N1 Zn1 141.54(17) . . ?
C4 N1 Zn1 111.53(14) . . ?
C9 N2 C5 120.00(19) . . ?
C9 N2 Zn1 129.53(16) . . ?
C5 N2 Zn1 110.43(14) . . ?
N1 C1 C2 110.3(2) . . ?
N1 C1 H1A 124.8 . . ?
C2 C1 H1A 124.8 . . ?
C1 C2 C3 106.8(2) . . ?
C1 C2 H2A 126.6 . . ?
C3 C2 H2A 126.6 . . ?
C4 C3 C2 106.5(2) . . ?
C4 C3 H3A 126.7 . . ?
C2 C3 H3A 126.7 . . ?
N1 C4 C3 109.5(2) . . ?
N1 C4 C5 118.05(19) . . ?
C3 C4 C5 132.4(2) . . ?
N2 C5 C6 119.9(2) . . ?
N2 C5 C4 115.59(19) . . ?
C6 C5 C4 124.5(2) . . ?
C7 C6 C5 119.6(2) . . ?
C7 C6 H6A 120.2 . . ?
C5 C6 H6A 120.2 . . ?
C6 C7 C8 119.9(2) . . ?
C6 C7 H7A 120.1 . . ?
C8 C7 H7A 120.1 . . ?
C9 C8 C7 118.4(2) . . ?
C9 C8 H8A 120.8 . . ?
C7 C8 H8A 120.8 . . ?
N2 C9 C8 122.2(2) . . ?
N2 C9 H9A 118.9 . . ?
C8 C9 H9A 118.9 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.055