Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2001


data_mp39-2

_database_code_CSD	160990

_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'Harrison, William T. A.'
'Nenoff, Tina M.'
'Phillips, Mark L. F.'

_publ_contact_author_name     	'Dr William T A Harrison'  
_publ_contact_author_address 
;
Dr William T A Harrison
Department of Chemistry
University of Aberdeen
Aberdeen
AB24 3UE
UNITED KINGDOM
;

_publ_contact_author_email       'W.HARRISON@ABDN.AC.UK'

_audit_creation_date        00-08-01
_audit_creation_method CRYSTALS_ver_07-07-97
_publ_requested_category   test
#  MP 39-2  transformed to Fdd2
#****************************************************************************
#==========================================================================

_chemical_name_systematic       # IUPAC name, in full
;
?
;
_chemical_melting_point                    'not measured'
_refine_ls_matrix_type                      full
_atom_sites_solution_primary                direct
# _atom_sites_solution_secondary            difmap
_atom_sites_solution_hydrogens              geom
_refine_ls_hydrogen_treatment               mixed
#****************************************************************************
_cell_length_a 15.2109(6)
_cell_angle_alpha 90.
_cell_length_b 11.7281(5)
_cell_angle_beta  90.
_cell_length_c 14.1821(6)
_cell_angle_gamma 90.
_cell_volume   2530.0
_symmetry_cell_setting 'Orthorhombic '
_symmetry_space_group_name_H-M 'F d d 2 '
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'x,y+1/2,z+1/2'
'x+1/2,y,z+1/2'
'x+1/2,y+1/2,z'
'-x+1/4,y+1/4,z+1/4'
'-x+1/4,y+3/4,z+3/4'
'-x+3/4,y+1/4,z+3/4'
'-x+3/4,y+3/4,z+1/4'
'x+1/4,-y+1/4,z+1/4'
'x+1/4,-y+3/4,z+3/4'
'x+3/4,-y+1/4,z+3/4'
'x+3/4,-y+3/4,z+1/4'
'-x+1/2,-y,z+1/2'
'-x+1/2,-y+1/2,z'
'-x,-y,z'
'-x,-y+1/2,z+1/2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'Zn  '    0.2220    1.4310   14.0743    3.2655
7.0318    0.2333    5.1652   10.3163    2.4100   58.7097    1.3041
'International_Tables_Vol_IV_Table_2.2B'
'P   '    0.0900    0.0950    6.4345    1.9067
4.1791   27.1570    1.7800    0.5260    1.4908   68.1645    1.1149
'International_Tables_Vol_IV_Table_2.2B'
'O   '    0.0080    0.0060    3.0485   13.2771
2.2868    5.7011    1.5463    0.3239    0.8670   32.9089    0.2508
'International_Tables_Vol_IV_Table_2.2B'
'N   '    0.0040    0.0030   12.2126    0.0057
3.1322    9.8933    2.0125   28.9975    1.1663    0.5826  -11.5290
'International_Tables_Vol_IV_Table_2.2B'
'C   '    0.0020    0.0020    2.3100   20.8439
1.0200   10.2075    1.5886    0.5687    0.8650   51.6512    0.2156
'International_Tables_Vol_IV_Table_2.2B'
'H   '    0.0000    0.0000    0.4930   10.5109
0.3229   26.1257    0.1402    3.1424    0.0408   57.7997    0.0030
'International_Tables_Vol_IV_Table_2.2B'
_chemical_formula_sum
' C2 H14 N6 O6 P2 Zn '
_chemical_formula_moiety
'(C N3 H6)2, Zn, (H P O3)2'
_chemical_compound_source
;
hydrothermal reaction
;
_diffrn_measurement_device_type 'Bruker SMART 1000'
_chemical_formula_weight   345.50
_cell_measurement_reflns_used        4902
_cell_measurement_theta_min        2.62
_cell_measurement_theta_max        32.48
_cell_measurement_temperature        298
_cell_formula_units_Z 8
_exptl_crystal_description ' octahedron '
_exptl_crystal_colour ' colourless '
_exptl_crystal_size_min 0.34
_exptl_crystal_size_mid 0.36
_exptl_crystal_size_max 0.36
_exptl_crystal_density_diffrn 1.81
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_F_000 1411.45
_exptl_absorpt_coefficient_mu 2.22
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min   0.809
_exptl_absorpt_correction_T_max   0.962 
_exptl_absorpt_process_details 'SADABS'

_diffrn_standards_interval_time 0
_diffrn_standards_interval_count 0
_diffrn_standards_number 0
_diffrn_standards_decay_% 0.00
_diffrn_ambient_temperature          298
_diffrn_reflns_number 6402
_reflns_number_total 2223
_diffrn_reflns_av_R_equivalents 0.02
# Number of reflections with Friedels Law is 0
# Number of reflections without Friedels Law is 2223
_reflns_number_gt 2131
_diffrn_reflns_theta_min 0.00
_diffrn_reflns_theta_max 32.50
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_limit_l_max 21
_reflns_limit_h_min 0
_reflns_limit_h_max 22
_reflns_limit_k_min 0
_reflns_limit_k_max 17
_reflns_limit_l_min -20
_reflns_limit_l_max 21
_reflns_threshold_expression  >1.00\s(I)
_refine_diff_density_min -0.52
_refine_diff_density_max 0.75
_refine_ls_number_reflns 2131
_refine_ls_number_parameters 84
_refine_ls_R_factor_gt 0.0203
_refine_ls_wR_factor_ref 0.0246
_refine_ls_goodness_of_fit_ref 1.03
_refine_ls_shift/su_max 0.0002
_refine_ls_abs_structure_Flack 0.037(7)
_refine_ls_abs_structure_details 'Flack, 2131 Friedel-pairs'
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Chebychev polynomial with   3 parameters (Carruthers & Watkin, 1979)
0.521 0.372 0.312
;
_diffrn_radiation_type       'Mo K\a'
_diffrn_radiation_wavelength      0.71073
_diffrn_measurement_method \w

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
Zn1 0.0000 0.0000 0.66938(3) 0.0188 1.0000 Uani
P1 0.168110(19) -0.12220(3) 0.59101(4) 0.0204 1.0000 Uani
O1 0.08797(8) -0.04633(12) 0.57837(9) 0.0374 1.0000 Uani
O2 0.22222(8) -0.11961(8) 0.49960(8) 0.0262 1.0000 Uani
O3 0.2218(1) -0.09656(13) 0.67659(9) 0.0394 1.0000 Uani
C1 0.13458(13) 0.13507(15) 0.36399(12) 0.0360 1.0000 Uani
N1 0.07277(14) 0.12854(17) 0.42840(14) 0.0536 1.0000 Uani
N2 0.20087(14) 0.06256(18) 0.36256(12) 0.0504 1.0000 Uani
N3 0.13132(13) 0.2154(2) 0.29818(15) 0.0554 1.0000 Uani
H1 0.1350(17) -0.226(2) 0.597(2) 0.0329 1.0000 Uiso
H11 0.07573 0.06803 0.47798 0.077(5) 1.0000 Uiso
H12 0.02318 0.18452 0.42839 0.077(5) 1.0000 Uiso
H21 0.20420 0.00044 0.41072 0.077(5) 1.0000 Uiso
H22 0.24760 0.06945 0.31329 0.077(5) 1.0000 Uiso
H31 0.17816 0.2194 0.24882 0.077(5) 1.0000 Uiso
H32 0.08265 0.2727 0.29861 0.077(5) 1.0000 Uiso
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 0.01984(8) 0.02054(8) 0.01609(8) 0.0000 0.0000 0.00016(7)
P1 0.02135(12) 0.02131(12) 0.01852(13) 0.0014(1) 0.0020(1) 0.00163(9)
O1 0.0335(5) 0.0499(7) 0.0288(5) 0.0115(5) 0.0111(4) 0.0204(5)
O2 0.0317(4) 0.0224(4) 0.0244(4) -0.0011(3) 0.0108(4) 0.0037(4)
O3 0.0414(6) 0.0499(7) 0.0269(6) -0.0042(5) -0.0085(5) -0.0039(5)
C1 0.0405(7) 0.0384(7) 0.0292(7) 0.0124(6) 0.0071(6) 0.0074(6)
N1 0.0600(11) 0.057(1) 0.0440(9) 0.0206(8) 0.0248(8) 0.0211(8)
N2 0.057(1) 0.058(1) 0.0371(8) 0.0157(7) 0.0121(7) 0.0257(9)
N3 0.0439(8) 0.0664(12) 0.0560(11) 0.039(1) 0.0124(8) 0.0156(8)
_refine_ls_extinction_coef 4.8(36)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 . O1 . 1.9370(11)    yes
Zn1 . O1 15_454 1.9370(11)    yes
Zn1 . O2 5_555 1.952(1)    yes
Zn1 . O2 12_445 1.952(1)    yes
P1 . O1 . 1.5198(11)    yes
P1 . O2 . 1.5358(11)    yes
P1 . O3 . 1.4935(13)    yes
P1 . H1 . 1.32(3)    no
C1 . N1 . 1.313(2)    yes
C1 . N2 . 1.319(2)    yes
C1 . N3 . 1.327(2)    yes
N1 . H11 . 1.000    no
N1 . H12 . 1.000    no
N2 . H21 . 1.000    no
N2 . H22 . 1.000    no
N3 . H31 . 1.000    no
N3 . H32 . 1.000    no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . Zn1 . O1 15_454 96.43(8)    yes
O1 . Zn1 . O2 5_555 117.29(6)    yes
O1 15_454 Zn1 . O2 5_555 108.55(5)    yes
O1 . Zn1 . O2 12_445 108.55(5)    yes
O1 15_454 Zn1 . O2 12_445 117.29(6)    yes
O2 5_555 Zn1 . O2 12_445 108.71(6)    yes
O1 . P1 . O2 . 108.58(6)    yes
O1 . P1 . O3 . 114.61(8)    yes
O2 . P1 . O3 . 112.89(7)    yes
O1 . P1 . H1 . 104.0(11)    no
O2 . P1 . H1 . 106.1(12)    no
O3 . P1 . H1 . 110.0(12)    no
Zn1 . O1 . P1 . 129.77(8)    yes
Zn1 6_544 O2 . P1 . 126.33(6)    yes
N1 . C1 . N2 . 121.36(16)    yes
N1 . C1 . N3 . 120.25(17)    yes
N2 . C1 . N3 . 118.39(17)    yes
C1 . N1 . H11 . 119.9(1)    no
C1 . N1 . H12 . 120.1(1)    no
H11 . N1 . H12 . 120.000    no
C1 . N2 . H21 . 119.9(1)    no
C1 . N2 . H22 . 120.1(1)    no
H21 . N2 . H22 . 120.000    no
C1 . N3 . H31 . 119.94(12)    no
C1 . N3 . H32 . 120.05(12)    no
H31 . N3 . H32 . 120.000    no

# end of file