# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

loop_
_publ_author_name
C.N.R.Rao
'Meenakshi Dan'
'D. Udayakumar'

_publ_contact_author_name        'Prof C N R Rao'
_publ_contact_author_address     
;
Chemistry and Physics of Materials Unit and
CSIR Centre of Excellence in Chemistry
Jawaharlal Nehru Centre for Advanced Scientific Research
Jakkar P O Bangalore
560064
INDIA
;

_publ_contact_author_email       CNRRAO@JNCASR.AC.IN

_publ_section_title              
;
Transformation of a 4-membered ring zinc phosphate
SBU to a sodalite structure through a linear chain structure
;

data_nikki
_database_code_CSD               212055

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C4 H16 N2 O9 P2 Zn'
_chemical_formula_weight         363.50
_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'
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'
P P 0.1023 0.0942 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   8.9088(15)
_cell_length_b                   14.030(2)
_cell_length_c                   9.3055(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.481(3)
_cell_angle_gamma                90.00
_cell_volume                     1157.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.085
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    2.442
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_correction_T_min  0.877944
_exptl_absorpt_correction_T_max  1.000000

_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       ?
_diffrn_measurement_method       ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4788
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         24.30
_reflns_number_total             1668
_reflns_number_observed          1262
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0266P)^2^+2.3519P] 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     SHELXL
_refine_ls_extinction_coef       0.0032(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         1668
_refine_ls_number_parameters     172
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_obs          0.0367
_refine_ls_wR_factor_all         0.0864
_refine_ls_wR_factor_obs         0.0769
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_obs   1.100
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.100
_refine_ls_shift/esd_max         0.001
_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
Zn1 Zn 1.00878(7) 1.03124(4) -0.23832(7) 0.0179(2) Uani 1 d . .
P1 P 0.78741(14) 1.08483(10) -0.00916(15) 0.0171(4) Uani 1 d . .
P2 P 1.17307(15) 1.08560(9) -0.51067(15) 0.0167(4) Uani 1 d . .
O1 O 0.8585(4) 1.1041(2) -0.1522(4) 0.0259(9) Uani 1 d . .
O2 O 1.0717(4) 1.0804(2) -0.6569(4) 0.0240(9) Uani 1 d . .
O3 O 1.1547(4) 1.0063(2) -0.0685(4) 0.0237(9) Uani 1 d . .
O4 O 1.0932(4) 1.1164(2) -0.3777(4) 0.0263(9) Uani 1 d . .
O5 O 0.7994(4) 1.1699(2) 0.0952(4) 0.0264(9) Uani 1 d . .
O6 O 0.6228(4) 1.0703(3) -0.0521(4) 0.0395(11) Uani 1 d . .
H2 H 0.6112(4) 1.0241(3) -0.1059(4) 0.059 Uiso 1 calc R .
O7 O 1.2596(4) 0.9957(3) -0.4841(4) 0.0260(9) Uani 1 d . .
H1 H 1.3240(4) 1.0031(3) -0.4160(4) 0.039 Uiso 1 calc R .
O8 O 1.2808(4) 1.1687(2) -0.5432(4) 0.0287(10) Uani 1 d . .
N1 N 0.2851(5) 1.3073(3) -1.1111(5) 0.0237(11) Uani 1 d . .
H14 H 0.3184(5) 1.3581(3) -1.0582(5) 0.028 Uiso 1 calc R .
H13 H 0.2849(5) 1.3225(3) -1.2051(5) 0.028 Uiso 1 calc R .
N2 N 0.2322(5) 1.1705(3) -0.8872(5) 0.0277(12) Uani 1 d . .
H12 H 0.2314(5) 1.1536(3) -0.7939(5) 0.033 Uiso 1 calc R .
H11 H 0.1992(5) 1.1206(3) -0.9423(5) 0.033 Uiso 1 calc R .
C1 C 0.3848(6) 1.2257(4) -1.0772(6) 0.0286(14) Uani 1 d . .
H10 H 0.4870(6) 1.2425(4) -1.0949(6) 0.034 Uiso 1 calc R .
H9 H 0.3529(6) 1.1727(4) -1.1398(6) 0.034 Uiso 1 calc R .
C2 C 0.1367(6) 1.2835(4) -1.0800(6) 0.0267(14) Uani 1 d . .
H8 H 0.0986(6) 1.2320(4) -1.1427(6) 0.032 Uiso 1 calc R .
H7 H 0.0713(6) 1.3382(4) -1.0992(6) 0.032 Uiso 1 calc R .
C3 C 0.3814(6) 1.1952(4) -0.9163(6) 0.0264(14) Uani 1 d . .
H6 H 0.4476(6) 1.1410(4) -0.8961(6) 0.032 Uiso 1 calc R .
H5 H 0.4178(6) 1.2472(4) -0.8537(6) 0.032 Uiso 1 calc R .
C4 C 0.1335(6) 1.2524(4) -0.9187(7) 0.0331(15) Uani 1 d . .
H4 H 0.1664(6) 1.3049(4) -0.8556(7) 0.040 Uiso 1 calc R .
H3 H 0.0312(6) 1.2359(4) -0.9007(7) 0.040 Uiso 1 calc R .
O100 O 1.5310(6) 1.0098(4) -0.3129(6) 0.057(2) Uani 1 d D .
H20 H 1.5801(77) 1.0161(51) -0.3764(76) 0.054(26) Uiso 1 d . .
H21 H 1.4509(31) 1.0022(41) -0.3558(55) 0.033(18) Uiso 1 d 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
Zn1 0.0182(3) 0.0164(4) 0.0198(4) 0.0002(3) 0.0053(2) 0.0008(3)
P1 0.0156(7) 0.0174(8) 0.0188(9) -0.0004(6) 0.0032(6) 0.0037(6)
P2 0.0172(7) 0.0147(8) 0.0187(8) 0.0000(6) 0.0054(6) -0.0019(6)
O1 0.028(2) 0.029(2) 0.023(2) 0.008(2) 0.011(2) 0.010(2)
O2 0.026(2) 0.022(2) 0.024(2) 0.001(2) -0.002(2) 0.000(2)
O3 0.020(2) 0.018(2) 0.034(2) 0.003(2) 0.002(2) 0.002(2)
O4 0.031(2) 0.021(2) 0.030(2) 0.001(2) 0.017(2) 0.000(2)
O5 0.035(2) 0.021(2) 0.024(2) -0.001(2) 0.007(2) 0.005(2)
O6 0.013(2) 0.061(3) 0.044(3) -0.008(2) 0.001(2) 0.002(2)
O7 0.020(2) 0.024(2) 0.033(2) 0.003(2) -0.002(2) 0.004(2)
O8 0.025(2) 0.024(2) 0.039(3) -0.004(2) 0.017(2) -0.010(2)
N1 0.034(3) 0.018(3) 0.019(3) 0.001(2) 0.007(2) -0.006(2)
N2 0.037(3) 0.024(3) 0.024(3) 0.005(2) 0.010(2) -0.005(2)
C1 0.024(3) 0.023(3) 0.041(4) 0.007(3) 0.012(3) -0.001(3)
C2 0.019(3) 0.022(3) 0.037(4) -0.003(3) -0.006(3) -0.001(2)
C3 0.021(3) 0.028(3) 0.029(4) 0.004(3) -0.005(3) 0.001(3)
C4 0.029(3) 0.025(3) 0.047(4) 0.001(3) 0.011(3) 0.000(3)
O100 0.024(3) 0.107(5) 0.038(3) -0.020(3) 0.000(2) -0.006(3)

_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 O1 1.920(3) . ?
Zn1 O2 1.945(4) 3_774 ?
Zn1 O4 1.965(3) . ?
Zn1 O3 1.979(3) . ?
P1 O6 1.497(4) . ?
P1 O3 1.534(4) 3_775 ?
P1 O5 1.536(4) . ?
P1 O1 1.551(4) . ?
P2 O7 1.487(4) . ?
P2 O4 1.547(4) . ?
P2 O8 1.558(4) . ?
P2 O2 1.561(4) . ?
O2 Zn1 1.945(4) 3_774 ?
O3 P1 1.534(4) 3_775 ?
N1 C2 1.420(6) . ?
N1 C1 1.464(6) . ?
N2 C3 1.425(6) . ?
N2 C4 1.460(7) . ?
C1 C3 1.561(8) . ?
C2 C4 1.566(8) . ?

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
O1 Zn1 O2 113.6(2) . 3_774 ?
O1 Zn1 O4 106.13(14) . . ?
O2 Zn1 O4 107.72(15) 3_774 . ?
O1 Zn1 O3 101.06(15) . . ?
O2 Zn1 O3 116.15(14) 3_774 . ?
O4 Zn1 O3 111.78(15) . . ?
O6 P1 O3 106.8(2) . 3_775 ?
O6 P1 O5 106.4(2) . . ?
O3 P1 O5 110.5(2) 3_775 . ?
O6 P1 O1 105.3(2) . . ?
O3 P1 O1 113.8(2) 3_775 . ?
O5 P1 O1 113.4(2) . . ?
O7 P2 O4 112.0(2) . . ?
O7 P2 O8 110.4(2) . . ?
O4 P2 O8 106.6(2) . . ?
O7 P2 O2 110.6(2) . . ?
O4 P2 O2 116.0(2) . . ?
O8 P2 O2 100.4(2) . . ?
P1 O1 Zn1 128.6(2) . . ?
P2 O2 Zn1 129.0(2) . 3_774 ?
P1 O3 Zn1 133.6(2) 3_775 . ?
P2 O4 Zn1 126.3(2) . . ?
C2 N1 C1 109.3(4) . . ?
C3 N2 C4 109.0(4) . . ?
N1 C1 C3 110.7(4) . . ?
N1 C2 C4 111.3(4) . . ?
N2 C3 C1 110.7(4) . . ?
N2 C4 C2 110.3(5) . . ?

_refine_diff_density_max         0.489
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.122