# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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data_compound1
_database_code_depnum_ccdc_archive 'CCDC 919221'
#TrackingRef 'Costantino_C1_C2_new.cif'
_audit_creation_method           'from EXP file using GSAS2CIF'
_refine_ls_shift/su_max          0.09
_refine_ls_shift/su_mean         0.02
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     66
_refine_ls_goodness_of_fit_all   3.24
_refine_ls_number_restraints     20
_refine_ls_matrix_type           full
_chemical_formula_moiety         ZrF2[(O3PCH2)2NHCH3]
_cell_measurement_temperature    298
#==============================================================================
# 8. Phase information from GSAS
_pd_phase_name                   1
_cell_length_a                   5.25279(9)
_cell_length_b                   8.5405(1)
_cell_length_c                   10.8457(2)
_cell_angle_alpha                84.869(1)
_cell_angle_beta                 88.183(1)
_cell_angle_gamma                72.651(1)
_cell_volume                     462.55(1)
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
-1 -x,-y,-z
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
Zr Zr1 1.0 1.0 0.0 1.0 Uiso 0.0174(10) 1
Zr Zr2 0.5 1.0 0.5 1.0 Uiso 0.0215(10) 1
P P1 0.5443(11) 0.8796(6) 0.1867(5) 1.0 Uiso 0.0228(17) 2
P P2 1.1533(10) 0.7296(7) 0.5353(5) 1.0 Uiso 0.0217(18) 2
F F3 0.9954(16) 0.7859(10) -0.0491(7) 1.0 Uiso 0.0235(13) 2
O O1 0.3055(18) 0.8710(12) 0.1217(9) 1.0 Uiso 0.0235(13) 2
O O2 1.2529(18) 0.6115(11) 0.4385(9) 1.0 Uiso 0.0235(13) 2
O O3 0.7036(19) 0.9727(14) 0.1179(8) 1.0 Uiso 0.0235(13) 2
O O4 1.3514(18) 0.8210(12) 0.5657(8) 1.0 Uiso 0.0235(13) 2
O O5 0.8859(17) 0.8625(12) 0.5049(9) 1.0 Uiso 0.0235(13) 2
O O6 0.4429(20) 0.9321(13) 0.3218(8) 1.0 Uiso 0.0235(13) 2
N N1 1.3096(22) 0.4654(14) 0.7261(12) 1.0 Uiso 0.0235(13) 2
C C1 1.4738(27) 0.5297(20) 0.8010(14) 1.0 Uiso 0.0235(13) 2
C C2 1.0721(27) 0.6050(16) 0.6720(11) 1.0 Uiso 0.0235(13) 2
C C3 0.7790(25) 0.6696(11) 0.2183(13) 1.0 Uiso 0.0235(13) 2
# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C3 F N O6 P2 Zr'
_chemical_formula_weight         318.20
_cell_formula_units_Z            2
# MOLECULAR GEOMETRY
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 F3 1.956(8) . 1_555 N
Zr1 F3 1.956(8) . -1_775 N
Zr1 O1 2.086(10) . 1_655 N
Zr1 O1 2.086(10) . -1_675 N
Zr1 O3 2.037(8) . 1_555 N
Zr1 O3 2.037(8) . -1_775 N
Zr2 O4 1.984(9) . 1_455 N
Zr2 O4 1.984(9) . -1_776 N
Zr2 O5 2.016(9) . 1_555 N
Zr2 O5 2.016(9) . -1_676 N
Zr2 O6 2.121(9) . 1_555 N
Zr2 O6 2.121(9) . -1_676 N
P1 O1 1.481(8) . 1_555 N
P1 O3 1.463(7) . 1_555 N
P1 O6 1.600(8) . 1_555 N
P1 C3 1.858(8) . 1_555 N
P2 O2 1.494(7) . 1_555 N
P2 O4 1.534(8) . 1_555 N
P2 O5 1.543(8) . 1_555 N
P2 C2 1.861(8) . 1_555 N
F3 Zr1 1.956(8) . 1_555 N
F3 O3 2.656(12) . 1_555 N
O1 Zr1 2.086(10) . 1_455 N
O1 P1 1.481(8) . 1_555 N
O1 O3 2.490(10) . 1_555 N
O1 O6 2.456(10) . 1_555 N
O2 P2 1.494(7) . 1_555 N
O2 O4 2.532(10) . 1_555 N
O2 O5 2.560(10) . 1_555 N
O2 N1 2.819(15) . -1_866 N
O3 Zr1 2.037(8) . 1_555 N
O3 P1 1.463(7) . 1_555 N
O3 F3 2.656(12) . 1_555 N
O3 O1 2.490(10) . 1_555 N
O3 O6 2.615(10) . 1_555 N
O4 Zr2 1.984(9) . 1_655 N
O4 P2 1.534(8) . 1_555 N
O4 O2 2.532(10) . 1_555 N
O4 O5 2.467(10) . 1_555 N
O4 O5 2.670(14) . -1_776 N
O5 Zr2 2.016(9) . 1_555 N
O5 P2 1.543(8) . 1_555 N
O5 O2 2.560(10) . 1_555 N
O5 O4 2.467(10) . 1_555 N
O5 O4 2.670(14) . -1_776 N
O6 Zr2 2.121(9) . 1_555 N
O6 P1 1.600(8) . 1_555 N
O6 O1 2.456(10) . 1_555 N
O6 O3 2.615(10) . 1_555 N
N1 O2 2.819(15) . -1_866 N
N1 C1 1.454(12) . 1_555 N
N1 C2 1.535(12) . 1_555 N
N1 C3 1.445(11) . -1_766 N
C1 N1 1.454(12) . 1_555 N
C2 P2 1.861(8) . 1_555 N
C2 N1 1.535(12) . 1_555 N
C3 P1 1.858(8) . 1_555 N
C3 N1 1.445(11) . -1_766 N
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F3 Zr1 F3 180.0 1_555 . -1_775 N
F3 Zr1 O1 87.01(32) 1_555 . 1_655 N
F3 Zr1 O1 92.99(32) 1_555 . -1_675 N
F3 Zr1 O3 83.4(4) 1_555 . 1_555 N
F3 Zr1 O3 96.6(4) 1_555 . -1_775 N
F3 Zr1 O1 92.99(32) -1_775 . 1_655 N
F3 Zr1 O1 87.01(32) -1_775 . -1_675 N
F3 Zr1 O3 96.6(4) -1_775 . 1_555 N
F3 Zr1 O3 83.4(4) -1_775 . -1_775 N
O1 Zr1 O1 180.0 1_655 . -1_675 N
O1 Zr1 O3 94.14(34) 1_655 . 1_555 N
O1 Zr1 O3 85.86(34) 1_655 . -1_775 N
O1 Zr1 O3 85.86(34) -1_675 . 1_555 N
O1 Zr1 O3 94.14(34) -1_675 . -1_775 N
O3 Zr1 O3 180.0 1_555 . -1_775 N
O4 Zr2 O4 180.0 1_455 . -1_776 N
O4 Zr2 O5 96.3(4) 1_455 . 1_555 N
O4 Zr2 O5 83.7(4) 1_455 . -1_676 N
O4 Zr2 O6 86.14(33) 1_455 . 1_555 N
O4 Zr2 O6 93.86(33) 1_455 . -1_676 N
O4 Zr2 O5 83.7(4) -1_776 . 1_555 N
O4 Zr2 O5 96.3(4) -1_776 . -1_676 N
O4 Zr2 O6 93.86(33) -1_776 . 1_555 N
O4 Zr2 O6 86.14(33) -1_776 . -1_676 N
O5 Zr2 O5 179.9604 1_555 . -1_676 N
O5 Zr2 O6 92.7(4) 1_555 . 1_555 N
O5 Zr2 O6 87.3(4) 1_555 . -1_676 N
O5 Zr2 O6 87.3(4) -1_676 . 1_555 N
O5 Zr2 O6 92.7(4) -1_676 . -1_676 N
O6 Zr2 O6 180.0 1_555 . -1_676 N
O1 P1 O3 115.5(7) 1_555 . 1_555 N
O1 P1 O6 105.6(6) 1_555 . 1_555 N
O1 P1 C3 110.0(7) 1_555 . 1_555 N
O3 P1 O6 117.2(6) 1_555 . 1_555 N
O3 P1 C3 104.5(7) 1_555 . 1_555 N
O6 P1 C3 103.2(7) 1_555 . 1_555 N
O2 P2 O4 113.5(6) 1_555 . 1_555 N
O2 P2 O5 114.9(6) 1_555 . 1_555 N
O2 P2 C2 105.4(7) 1_555 . 1_555 N
O4 P2 O5 106.6(6) 1_555 . 1_555 N
O4 P2 C2 112.6(7) 1_555 . 1_555 N
O5 P2 C2 103.6(6) 1_555 . 1_555 N
Zr1 O1 P1 144.4(6) 1_455 . 1_555 N
Zr1 O3 P1 154.6(8) 1_555 . 1_555 N
Zr2 O4 P2 142.3(6) 1_655 . 1_555 N
Zr2 O5 P2 164.8(7) 1_555 . 1_555 N
Zr2 O6 P1 152.7(6) 1_555 . 1_555 N
C1 N1 C2 110.6(9) 1_555 . 1_555 N
C1 N1 C3 117.4(11) 1_555 . -1_766 N
C2 N1 C3 110.5(9) 1_555 . -1_766 N
_diffrn_ambient_temperature      298
loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Zr 2.0 -0.314 2.245 17.8765 1.27618 10.9480 11.9160 5.41732 0.11762 3.65721
87.6627 2.06929 International_Tables_Vol_C
P 4.0 0.283 0.434 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080
68.1645 1.11490 International_Tables_Vol_C
F 2.0 0.069 0.053 3.53920 10.2825 2.64120 4.29440 1.51700 0.26150 1.02430
26.1476 0.27760 International_Tables_Vol_C
O 12.0 0.047 0.032 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
N 2.0 0.029 0.018 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630
0.58260 -11.529 International_Tables_Vol_C
C 6.0 0.017 0.009 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500
51.6512 0.21560 International_Tables_Vol_C
_diffrn_radiation_probe          x-ray
_diffrn_radiation_polarisn_ratio 0.75
loop_
_diffrn_radiation_wavelength
_diffrn_radiation_wavelength_wt
_diffrn_radiation_type
_diffrn_radiation_wavelength_id
1.540500 1.000 K\a~1~ 1
1.544300 0.500 K\a~2~ 2
_pd_proc_ls_prof_R_factor        0.0828
_pd_proc_ls_prof_wR_factor       0.1060
_pd_proc_ls_prof_wR_expected     0.0336
_refine_ls_R_Fsqd_factor         0.08601
_pd_proc_ls_background_function  
; GSAS Background function number 1 with 12 terms.
Shifted Chebyshev function of 1st kind
1: 320.059 2: -48.2585 3: 80.1247 4: 7.90565
5: -1.38748 6: 10.9692 7: -9.34426 8: 24.1782
9: -23.0867 10: -1.16022 11: 3.32297 12: -13.1886
;
_exptl_absorpt_process_details   
; GSAS Absorption/surface roughness correction: function number 0
No correction is applied.
;
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_T_max  1.00000
# Extinction correction
_gsas_exptl_extinct_corr_T_min   1.00000
_gsas_exptl_extinct_corr_T_max   1.00000
_pd_proc_ls_pref_orient_corr     
; March-Dollase
AXIS 1 Ratio= 0.93840 h= 1.000 k= 2.000 l= 0.000
Prefered orientation correction range: Min= 0.90903, Max= 1.21016
;
_pd_proc_ls_profile_function     
;
CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 25.522 #2(GV) = -2.000 #3(GW) = 0.875
#4(GP) = 0.100 #5(LX) = 0.833 #6(LY) = 14.114
#7(S/L) = 0.0217 #8(H/L) = 0.0294
#9(trns) = 0.00 #10(shft)= 0.0000
#11(stec)= 0.00 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000
#17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000
Peak tails are ignored where the intensity is below 0.0050 times the peak
Aniso. broadening axis 0.0 0.0 1.0
;
_pd_proc_ls_peak_cutoff          0.00500
_pd_proc_info_datetime           2011-12-12T11:01:33
_pd_calc_method                  'Rietveld Refinement'
#---- raw/calc data loop -----
_pd_meas_2theta_range_min        5.0
_pd_meas_2theta_range_max        140.0
_pd_meas_2theta_range_inc        0.02
_pd_proc_2theta_range_min        4.99129
_pd_proc_2theta_range_max        139.99129
_pd_proc_2theta_range_inc        0.02
_reflns_number_total             3103
_reflns_limit_h_min              0
_reflns_limit_h_max              6
_reflns_limit_k_min              -9
_reflns_limit_k_max              10
_reflns_limit_l_min              -12
_reflns_limit_l_max              12
_reflns_d_resolution_high        0.850
_reflns_d_resolution_low         6.246
_chemical_name_common            1


data_compound2
_database_code_depnum_ccdc_archive 'CCDC 919222'
#TrackingRef 'Costantino_C1_C2_new.cif'
_audit_creation_method           'from EXP file using GSAS2CIF'
_refine_ls_shift/su_max          0.07
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     64
_refine_ls_goodness_of_fit_all   3.11
_refine_ls_number_restraints     38
_refine_ls_matrix_type           full
_chemical_formula_moiety         Zr[(HO3PCH2)(O3PCH2)NHC2H5]2
_cell_measurement_temperature    298
#==============================================================================
# 8. Phase information from GSAS
_pd_phase_name                   2
_cell_length_a                   14.02463(7)
_cell_length_b                   14.02463
_cell_length_c                   25.0329(2)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_volume                     4264.08(4)
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3'
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -y,x-y,+z
3 y-x,-x,+z
-1 -x,-y,-z
-2 +y,y-x,-z
-3 x-y,+x,-z
101 +x+1/3,+y+2/3,+z+2/3
102 -y+1/3,x-y+2/3,+z+2/3
103 y-x+1/3,-x+2/3,+z+2/3
-101 -x+2/3,-y+1/3,-z+1/3
-102 +y+2/3,y-x+1/3,-z+1/3
-103 x-y+2/3,+x+1/3,-z+1/3
201 +x+2/3,+y+1/3,+z+1/3
202 -y+2/3,x-y+1/3,+z+1/3
203 y-x+2/3,-x+1/3,+z+1/3
-201 -x+1/3,-y+2/3,-z+2/3
-202 +y+1/3,y-x+2/3,-z+2/3
-203 x-y+1/3,+x+2/3,-z+2/3
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
C C(1) 0.4588(10) -0.1068(8) 0.1012(4) 1.0 Uiso 0.0265(9) 18
C C(2) 0.5490(8) 0.0024(9) 0.0860(5) 1.0 Uiso 0.0265(9) 18
N N(1) 0.6509(7) -0.0033(8) 0.0700(5) 1.0 Uiso 0.0265(9) 18
C C(3) 0.7104(9) -0.0146(9) 0.1111(5) 1.0 Uiso 0.0265(9) 18
C C(4) 0.7276(8) 0.0897(8) 0.0340(5) 1.0 Uiso 0.0265(9) 18
P P(1) 0.79425(27) -0.08350(30) 0.09565(16) 1.0 Uiso 0.0227(11) 18
P P(2) 0.81115(30) 0.23458(28) 0.05953(15) 1.0 Uiso 0.0262(12) 18
O O(1) 0.8639(5) -0.0584(7) 0.14406(26) 1.0 Uiso 0.0265(9) 18
O O(2) 0.7172(6) -0.2015(6) 0.08248(35) 1.0 Uiso 0.0265(9) 18
O O(3) 0.8671(5) -0.0285(5) 0.04729(24) 1.0 Uiso 0.0265(9) 18
O O(4) 0.8973(6) 0.2396(5) 0.10347(32) 1.0 Uiso 0.0265(9) 18
O O(5) 0.8630(6) 0.3055(6) 0.01144(31) 1.0 Uiso 0.0265(9) 18
O O(6) 0.7364(7) 0.2634(7) 0.09223(31) 1.0 Uiso 0.0265(9) 18
Zr Zr(1) 0.6667 0.3333 0.13854(7) 1.0 Uiso 0.0092(5) 6
Zr Zr(2) 1.0 0.0 0.0 1.0 Uiso 0.0163(8) 3
# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C8 N2 O12 P4 Zr'
_chemical_formula_weight         531.21
_cell_formula_units_Z            9
# MOLECULAR GEOMETRY
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C(1) C(2) 1.467(11) . 1_555 N
N(1) C(2) 1.524(11) . 1_555 N
N(1) C(3) 1.384(11) . 1_555 N
N(1) C(4) 1.506(11) . 1_555 N
P(1) C(3) 1.898(9) . 1_555 N
P(1) O(1) 1.485(6) . 1_555 N
P(1) O(2) 1.492(7) . 1_555 N
P(1) O(3) 1.522(6) . 1_555 N
P(2) C(4) 1.879(9) . 1_555 N
P(2) O(4) 1.610(7) . 1_555 N
P(2) O(5) 1.498(7) . 1_555 N
P(2) O(6) 1.535(6) . 1_555 N
Zr(1) O(1) 2.088(6) . -102_565 N
Zr(1) O(1) 2.089(6) . -101_655 N
Zr(1) O(1) 2.088(6) . -103_445 N
Zr(1) O(6) 2.054(6) . 1_555 N
Zr(1) O(6) 2.055(6) . 2_655 N
Zr(1) O(6) 2.055(6) . 3_665 N
Zr(2) O(3) 2.072(5) . 1_555 N
Zr(2) O(3) 2.072(5) . 2_645 N
Zr(2) O(3) 2.072(5) . 3_765 N
Zr(2) O(3) 2.072(5) . -1_755 N
Zr(2) O(3) 2.072(5) . -2_665 N
Zr(2) O(3) 2.072(5) . -3_545 N
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C(1) C(2) N(1) 110.8(10) 1_555 . 1_555 N
C(2) N(1) C(3) 116.4(10) 1_555 . 1_555 N
C(2) N(1) C(4) 113.3(9) 1_555 . 1_555 N
C(3) N(1) C(4) 109.5(9) 1_555 . 1_555 N
N(1) C(3) P(1) 118.0(9) 1_555 . 1_555 N
N(1) C(4) P(2) 121.5(9) 1_555 . 1_555 N
C(3) P(1) O(1) 102.4(5) 1_555 . 1_555 N
C(3) P(1) O(2) 108.6(5) 1_555 . 1_555 N
C(3) P(1) O(3) 109.5(5) 1_555 . 1_555 N
O(1) P(1) O(2) 118.0(5) 1_555 . 1_555 N
O(1) P(1) O(3) 109.5(4) 1_555 . 1_555 N
O(2) P(1) O(3) 108.5(5) 1_555 . 1_555 N
C(4) P(2) O(4) 109.2(5) 1_555 . 1_555 N
C(4) P(2) O(5) 106.1(5) 1_555 . 1_555 N
C(4) P(2) O(6) 109.1(5) 1_555 . 1_555 N
O(4) P(2) O(5) 114.5(4) 1_555 . 1_555 N
O(4) P(2) O(6) 102.8(4) 1_555 . 1_555 N
O(5) P(2) O(6) 115.0(5) 1_555 . 1_555 N
P(1) O(3) Zr(2) 149.7(5) 1_555 . 1_555 N
P(2) O(6) Zr(1) 167.8(6) 1_555 . 1_555 N
O(1) Zr(1) O(1) 86.85(28) -101_655 . -102_565 N
O(1) Zr(1) O(1) 86.88(28) -101_655 . -103_445 N
O(1) Zr(1) O(6) 88.36(31) -101_655 . 1_555 N
O(1) Zr(1) O(6) 93.56(28) -101_655 . 2_655 N
O(1) Zr(1) O(6) 175.17(34) -101_655 . 3_665 N
O(1) Zr(1) O(1) 86.85(28) -102_565 . -103_445 N
O(1) Zr(1) O(6) 175.17(34) -102_565 . 1_555 N
O(1) Zr(1) O(6) 88.31(31) -102_565 . 2_655 N
O(1) Zr(1) O(6) 93.53(28) -102_565 . 3_665 N
O(1) Zr(1) O(6) 93.59(28) -103_445 . 1_555 N
O(1) Zr(1) O(6) 175.11(34) -103_445 . 2_655 N
O(1) Zr(1) O(6) 88.33(31) -103_445 . 3_665 N
O(6) Zr(1) O(6) 91.29(31) 1_555 . 2_655 N
O(6) Zr(1) O(6) 91.29(31) 1_555 . 3_665 N
O(6) Zr(1) O(6) 91.26(31) 2_655 . 3_665 N
O(3) Zr(2) O(3) 90.59(24) 1_555 . 2_645 N
O(3) Zr(2) O(3) 90.59(24) 1_555 . 3_765 N
O(3) Zr(2) O(3) 180.0 1_555 . -1_755 N
O(3) Zr(2) O(3) 89.41(24) 1_555 . -2_665 N
O(3) Zr(2) O(3) 89.41(24) 1_555 . -3_545 N
O(3) Zr(2) O(3) 90.59(24) 2_645 . 3_765 N
O(3) Zr(2) O(3) 89.41(24) 2_645 . -1_755 N
O(3) Zr(2) O(3) 179.9802 2_645 . -2_665 N
O(3) Zr(2) O(3) 89.41(24) 2_645 . -3_545 N
O(3) Zr(2) O(3) 89.41(24) 3_765 . -1_755 N
O(3) Zr(2) O(3) 89.41(24) 3_765 . -2_665 N
O(3) Zr(2) O(3) 180.0 3_765 . -3_545 N
O(3) Zr(2) O(3) 90.59(24) -1_755 . -2_665 N
O(3) Zr(2) O(3) 90.59(24) -1_755 . -3_545 N
O(3) Zr(2) O(3) 90.59(24) -2_665 . -3_545 N
_diffrn_ambient_temperature      298
loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 72.0 0.017 0.009 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500
51.6512 0.21560 International_Tables_Vol_C
N 18.0 0.029 0.018 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630
0.58260 -11.529 International_Tables_Vol_C
P 36.0 0.283 0.434 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080
68.1645 1.11490 International_Tables_Vol_C
O 108.0 0.047 0.032 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
Zr 9.0 -0.314 2.245 17.8765 1.27618 10.9480 11.9160 5.41732 0.11762 3.65721
87.6627 2.06929 International_Tables_Vol_C
_diffrn_radiation_probe          x-ray
_diffrn_radiation_polarisn_ratio 0.75
loop_
_diffrn_radiation_wavelength
_diffrn_radiation_wavelength_wt
_diffrn_radiation_type
_diffrn_radiation_wavelength_id
1.540500 1.000 K\a~1~ 1
1.544300 0.500 K\a~2~ 2
_pd_proc_ls_prof_R_factor        0.0734
_pd_proc_ls_prof_wR_factor       0.0966
_pd_proc_ls_prof_wR_expected     0.0317
_refine_ls_R_Fsqd_factor         0.06880
_pd_proc_ls_background_function  
; GSAS Background function number 1 with 12 terms.
Shifted Chebyshev function of 1st kind
1: 290.200 2: 10.5711 3: 40.1096 4: 21.9982
5: 8.03401 6: -20.7791 7: 6.88633 8: -11.2947
9: -2.24273 10: -5.61902 11: 1.85880 12: 1.54705
;
_exptl_absorpt_process_details   
; GSAS Absorption/surface roughness correction: function number 0
No correction is applied.
;
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_T_max  1.00000
# Extinction correction
_gsas_exptl_extinct_corr_T_min   1.00000
_gsas_exptl_extinct_corr_T_max   1.00000
_pd_proc_ls_pref_orient_corr     
; March-Dollase
AXIS 1 Ratio= 0.75962 h= 1.000 k= 0.000 l= 1.000
Prefered orientation correction range: Min= 0.78487, Max= 1.21892
;
_pd_proc_ls_profile_function     
;
CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 20.463 #2(GV) = 0.000 #3(GW) = 1.305
#4(GP) = 0.000 #5(LX) = 1.367 #6(LY) = 5.498
#7(S/L) = 0.0302 #8(H/L) = 0.0267
#9(trns) = 0.00 #10(shft)= 0.0000
#11(stec)= 0.00 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000
#17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000
Peak tails are ignored where the intensity is below 0.0005 times the peak
Aniso. broadening axis 0.0 0.0 1.0
;
_pd_proc_ls_peak_cutoff          0.00050
_pd_proc_info_datetime           2011-12-06T09:39:27
_pd_calc_method                  'Rietveld Refinement'
#---- raw/calc data loop -----
_pd_meas_2theta_range_min        3.0
_pd_meas_2theta_range_max        140.0
_pd_meas_2theta_range_inc        0.02
_pd_proc_2theta_range_min        2.99508
_pd_proc_2theta_range_max        139.99507
_pd_proc_2theta_range_inc        0.02
_reflns_number_total             3564
_reflns_limit_h_min              0
_reflns_limit_h_max              17
_reflns_limit_k_min              -8
_reflns_limit_k_max              8
_reflns_limit_l_min              -30
_reflns_limit_l_max              30
_reflns_d_resolution_high        0.822
_reflns_d_resolution_low         8.716
#--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#
_chemical_name_common            2