# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Ramaswamy Murugavel'
_publ_contact_author_address     
;
Chemistry
IIT-Bombay
Powai
Mumbai
400076
INDIA
;

_publ_contact_author_email       RMV@CHEM.IITB.AC.IN

_publ_section_title              
;
Seeking tetrameric transition metal phosphonate with a
D4R core and Organising it into a 3-D supramolecular assembly
;
loop_
_publ_author_name
'Ramaswamy Murugavel'
'Swaminathan Shanmugan'

# Attachment 'newrm060.cif'

data_newrm060
_database_code_depnum_ccdc_archive 'CCDC 626721'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H60 N8 O12 P4 Zn4'
_chemical_formula_sum            'C36 H60 N8 O12 P4 Zn4'
_chemical_formula_weight         1182.28

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'
Zn Zn 0.2839 1.4301 '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'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   20.1904(2)
_cell_length_b                   20.1904(2)
_cell_length_c                   12.8455(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5236.50(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2432
_exptl_absorpt_coefficient_mu    1.992
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.5593
_exptl_absorpt_correction_T_max  0.7156
_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            15034
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2303
_reflns_number_gt                1913
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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^)+(0.0577P)^2^+9.0036P] 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_number_reflns         2303
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.1050
_refine_ls_wR_factor_gt          0.0957
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.000
_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 0.459762(17) 0.152228(16) 0.49493(3) 0.03097(16) Uani 1 1 d . . .
P1 P 0.60725(4) 0.19818(4) 0.50220(6) 0.0287(2) Uani 1 1 d . . .
O1 O 0.55426(11) 0.14537(10) 0.52064(19) 0.0382(5) Uani 1 1 d . . .
O2 O 0.58238(12) 0.26621(11) 0.5302(2) 0.0456(6) Uani 1 1 d . . .
O3 O 0.63442(11) 0.19422(12) 0.39209(19) 0.0434(6) Uani 1 1 d . . .
N1 N 0.41350(13) 0.08932(12) 0.5959(2) 0.0372(6) Uani 1 1 d . . .
N2 N 0.42252(18) -0.00213(15) 0.4903(3) 0.0539(9) Uani 1 1 d . . .
H2A H 0.4405 0.0227 0.4439 0.065 Uiso 1 1 calc R . .
H2B H 0.4169 -0.0436 0.4783 0.065 Uiso 1 1 calc R . .
C1 C 0.67653(18) 0.17826(17) 0.5880(3) 0.0465(9) Uani 1 1 d . . .
C3 C 0.7090(2) 0.1127(2) 0.5547(5) 0.0743(15) Uani 1 1 d . . .
H3A H 0.7243 0.1164 0.4841 0.111 Uiso 1 1 calc R . .
H3B H 0.6772 0.0775 0.5596 0.111 Uiso 1 1 calc R . .
H3C H 0.7459 0.1033 0.5996 0.111 Uiso 1 1 calc R . .
C2 C 0.6519(3) 0.1729(3) 0.6998(4) 0.0847(16) Uani 1 1 d . . .
H2C H 0.6316 0.2139 0.7200 0.127 Uiso 1 1 calc R . .
H2D H 0.6885 0.1636 0.7451 0.127 Uiso 1 1 calc R . .
H2E H 0.6199 0.1378 0.7046 0.127 Uiso 1 1 calc R . .
C4 C 0.7286(2) 0.2336(2) 0.5808(4) 0.0740(14) Uani 1 1 d . . .
H4A H 0.7441 0.2371 0.5103 0.111 Uiso 1 1 calc R . .
H4B H 0.7651 0.2234 0.6259 0.111 Uiso 1 1 calc R . .
H4C H 0.7090 0.2749 0.6016 0.111 Uiso 1 1 calc R . .
C5 C 0.40338(16) 0.02379(15) 0.5812(3) 0.0388(8) Uani 1 1 d . . .
C6 C 0.3728(2) -0.01496(18) 0.6586(4) 0.0553(10) Uani 1 1 d . . .
H6 H 0.3668 -0.0601 0.6482 0.066 Uiso 1 1 calc R . .
C7 C 0.3524(2) 0.0134(2) 0.7476(4) 0.0643(12) Uani 1 1 d . . .
H7 H 0.3311 -0.0118 0.7981 0.077 Uiso 1 1 calc R . .
C8 C 0.3632(2) 0.0807(2) 0.7641(3) 0.0615(11) Uani 1 1 d . . .
H8 H 0.3501 0.1009 0.8259 0.074 Uiso 1 1 calc R . .
C9 C 0.3934(2) 0.11612(18) 0.6872(3) 0.0494(9) Uani 1 1 d . . .
H9 H 0.4006 0.1611 0.6980 0.059 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 0.0337(2) 0.0221(2) 0.0371(3) 0.00016(14) 0.00032(15) -0.00256(13)
P1 0.0317(4) 0.0212(4) 0.0331(5) 0.0019(3) -0.0070(3) -0.0002(3)
O1 0.0358(12) 0.0255(11) 0.0534(15) 0.0037(10) -0.0056(10) -0.0022(9)
O2 0.0547(15) 0.0243(11) 0.0579(16) -0.0006(10) -0.0067(12) 0.0035(10)
O3 0.0345(12) 0.0583(15) 0.0375(14) 0.0016(11) -0.0025(10) 0.0074(11)
N1 0.0410(15) 0.0266(13) 0.0439(17) 0.0046(12) 0.0017(13) -0.0003(11)
N2 0.069(2) 0.0256(15) 0.067(2) -0.0006(14) 0.0112(17) -0.0044(14)
C1 0.049(2) 0.0396(19) 0.051(2) 0.0096(16) -0.0224(17) -0.0081(15)
C3 0.061(3) 0.051(2) 0.111(4) 0.004(3) -0.046(3) 0.0144(19)
C2 0.106(4) 0.098(4) 0.050(3) 0.018(3) -0.029(3) -0.010(3)
C4 0.058(3) 0.063(3) 0.101(4) 0.011(3) -0.039(3) -0.020(2)
C5 0.0345(17) 0.0290(16) 0.053(2) 0.0065(15) -0.0044(15) -0.0005(13)
C6 0.062(2) 0.0364(19) 0.068(3) 0.0197(19) -0.004(2) -0.0107(17)
C7 0.066(3) 0.062(3) 0.064(3) 0.027(2) 0.010(2) -0.008(2)
C8 0.072(3) 0.062(3) 0.051(3) 0.007(2) 0.017(2) 0.007(2)
C9 0.065(2) 0.0387(19) 0.045(2) 0.0053(16) 0.0096(18) 0.0019(17)

_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 O2 1.908(2) 2_655 ?
Zn1 O3 1.935(2) 11_666 ?
Zn1 O1 1.941(2) . ?
Zn1 N1 2.041(3) . ?
P1 O2 1.506(2) . ?
P1 O3 1.519(2) . ?
P1 O1 1.529(2) . ?
P1 C1 1.826(3) . ?
O2 Zn1 1.908(2) 2_655 ?
O3 Zn1 1.935(2) 12_656 ?
N1 C5 1.352(4) . ?
N1 C9 1.354(5) . ?
N2 C5 1.337(5) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
C1 C2 1.523(6) . ?
C1 C4 1.537(5) . ?
C1 C3 1.538(6) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C2 H2C 0.9600 . ?
C2 H2D 0.9600 . ?
C2 H2E 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.407(5) . ?
C6 C7 1.344(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.392(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.364(6) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?

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
O2 Zn1 O3 118.26(11) 2_655 11_666 ?
O2 Zn1 O1 117.35(10) 2_655 . ?
O3 Zn1 O1 106.67(10) 11_666 . ?
O2 Zn1 N1 100.50(11) 2_655 . ?
O3 Zn1 N1 105.41(10) 11_666 . ?
O1 Zn1 N1 107.30(10) . . ?
O2 P1 O3 112.98(15) . . ?
O2 P1 O1 111.46(14) . . ?
O3 P1 O1 111.11(14) . . ?
O2 P1 C1 108.20(16) . . ?
O3 P1 C1 105.90(16) . . ?
O1 P1 C1 106.80(15) . . ?
P1 O1 Zn1 127.71(13) . . ?
P1 O2 Zn1 151.56(19) . 2_655 ?
P1 O3 Zn1 134.45(14) . 12_656 ?
C5 N1 C9 117.8(3) . . ?
C5 N1 Zn1 126.1(2) . . ?
C9 N1 Zn1 116.0(2) . . ?
C5 N2 H2A 120.0 . . ?
C5 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C2 C1 C4 109.4(4) . . ?
C2 C1 C3 109.9(4) . . ?
C4 C1 C3 108.5(4) . . ?
C2 C1 P1 109.5(3) . . ?
C4 C1 P1 109.1(3) . . ?
C3 C1 P1 110.4(3) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C2 H2C 109.5 . . ?
C1 C2 H2D 109.5 . . ?
H2C C2 H2D 109.5 . . ?
C1 C2 H2E 109.5 . . ?
H2C C2 H2E 109.5 . . ?
H2D C2 H2E 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 N1 117.4(3) . . ?
N2 C5 C6 121.8(3) . . ?
N1 C5 C6 120.8(3) . . ?
C7 C6 C5 119.9(4) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 119.8(4) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C9 C8 C7 118.1(4) . . ?
C9 C8 H8 120.9 . . ?
C7 C8 H8 120.9 . . ?
N1 C9 C8 123.5(4) . . ?
N1 C9 H9 118.2 . . ?
C8 C9 H9 118.2 . . ?

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
O2 P1 O1 Zn1 38.5(2) . . . . ?
O3 P1 O1 Zn1 -88.4(2) . . . . ?
C1 P1 O1 Zn1 156.52(19) . . . . ?
O2 Zn1 O1 P1 -40.5(2) 2_655 . . . ?
O3 Zn1 O1 P1 94.82(19) 11_666 . . . ?
N1 Zn1 O1 P1 -152.61(18) . . . . ?
O3 P1 O2 Zn1 35.3(4) . . . 2_655 ?
O1 P1 O2 Zn1 -90.6(4) . . . 2_655 ?
C1 P1 O2 Zn1 152.2(3) . . . 2_655 ?
O2 P1 O3 Zn1 -59.7(3) . . . 12_656 ?
O1 P1 O3 Zn1 66.5(2) . . . 12_656 ?
C1 P1 O3 Zn1 -177.9(2) . . . 12_656 ?
O2 Zn1 N1 C5 152.3(3) 2_655 . . . ?
O3 Zn1 N1 C5 28.9(3) 11_666 . . . ?
O1 Zn1 N1 C5 -84.6(3) . . . . ?
O2 Zn1 N1 C9 -30.1(3) 2_655 . . . ?
O3 Zn1 N1 C9 -153.5(3) 11_666 . . . ?
O1 Zn1 N1 C9 93.0(3) . . . . ?
O2 P1 C1 C2 65.4(3) . . . . ?
O3 P1 C1 C2 -173.2(3) . . . . ?
O1 P1 C1 C2 -54.7(3) . . . . ?
O2 P1 C1 C4 -54.4(4) . . . . ?
O3 P1 C1 C4 67.0(3) . . . . ?
O1 P1 C1 C4 -174.5(3) . . . . ?
O2 P1 C1 C3 -173.5(3) . . . . ?
O3 P1 C1 C3 -52.1(3) . . . . ?
O1 P1 C1 C3 66.4(3) . . . . ?
C9 N1 C5 N2 179.1(3) . . . . ?
Zn1 N1 C5 N2 -3.3(4) . . . . ?
C9 N1 C5 C6 0.1(5) . . . . ?
Zn1 N1 C5 C6 177.6(3) . . . . ?
N2 C5 C6 C7 -177.8(4) . . . . ?
N1 C5 C6 C7 1.1(6) . . . . ?
C5 C6 C7 C8 -1.8(7) . . . . ?
C6 C7 C8 C9 1.3(7) . . . . ?
C5 N1 C9 C8 -0.6(6) . . . . ?
Zn1 N1 C9 C8 -178.4(3) . . . . ?
C7 C8 C9 N1 -0.1(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.079