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


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data_ZBP-K
_database_code_depnum_ccdc_archive 'CCDC 916295'
#TrackingRef 'web_deposit_cif_file_0_KazuyukiMaeda_1355832349.ZBPs_submission3.cif'
# 5. CHEMICAL DATA
_chemical_name_common            ZBP-K
_chemical_formula_moiety         'C12 H6 K2 O21 P6 Zn5'
_chemical_formula_sum            'C12 H12 K2 O21 P6 Zn5'
_chemical_formula_weight         1083.150
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn -0.3771 2.5535 'International Tables for Crystallography, Vol. C'
K K 0.2812 0.4797 'International Tables for Crystallography, Vol. C'
P P 0.1621 0.1866 'International Tables for Crystallography, Vol. C'
O O 0.0196 0.0127 'International Tables for Crystallography, Vol. C'
C C 0.0064 0.0035 'International Tables for Crystallography, Vol. C'
H H 0.0000 0.0000 'International Tables for Crystallography, Vol. C'
# 6. POWDER SPECIMEN AND CRYSTAL DATA
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'I b a 2'
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_Int_Tables_number      45
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,z
3 x+1/2,-y+1/2,z
4 -x+1/2,y+1/2,z
5 x+1/2,y+1/2,z+1/2
6 -x+1/2,-y+1/2,z+1/2
7 x,-y,z+1/2
8 -x,y,z+1/2
_cell_length_a                   8.4899(1)
_cell_length_b                   16.1856(3)
_cell_length_c                   19.8846(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2732.44(8)
_cell_formula_units_Z            4
_exptl_crystal_density_diffrn    2.6330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2120.00
_pd_spec_mounting                'Lindemann glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_colour                  colorless
# 7. EXPERIMENTAL DATA
_diffrn_ambient_temperature      300
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  Debye-Scherrer
_diffrn_detector                 'imaging plate'
_pd_meas_scan_method             fixed
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.99752
_pd_meas_number_of_points        7101
_pd_meas_2theta_range_min        3.0000
_pd_meas_2theta_range_max        74.0000
_pd_meas_2theta_range_inc        0.0100
# 8. REFINEMENT DATA
_pd_proc_ls_special_details      
; Anisotropic line broadening factors Ue and Pe were refined.
;
_pd_calc_method                  'Rietveld Refinement'
_pd_proc_ls_profile_function     'split pseudo-Voigt function'
_pd_proc_ls_background_function  'Legendre polynomials'
_pd_proc_ls_pref_orient_corr     
; ?
;
#; $P_k = \sum_{j=1}^{m_k} \frac{1}{m_k}
#\left( r^2 \cos^2 \alpha_j +r^{-1}\ sin^2 \alpha_j \right)^{-3/2}$
#with a preferred-orientation vector, (hkl),
#and <i>r</i> = 1.0(0)
_pd_proc_ls_prof_R_factor        0.00601
_pd_proc_ls_prof_wR_factor       0.00783
_pd_proc_ls_prof_wR_expected     0.00730
_refine_ls_R_I_factor            0.01782
_refine_ls_R_Fsqd_factor         0.01526
_refine_ls_R_factor_all          0.01529
_refine_special_details          
; A virtual chemical species Ow (1O and 2H) is introduced
for Ow1 and Ow2 to simulate water molecules.
;
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/<i>y</i>~i~
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_parameters     111
_refine_ls_number_restraints     97
_refine_ls_number_constraints    20
# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   1.0719
_refine_ls_shift/su_max          0.0
#_refine_diff_density_max 0.0
#_refine_diff_density_min 0.0
# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.
_pd_proc_2theta_range_min        4.5000
_pd_proc_2theta_range_max        65.0000
_pd_proc_2theta_range_inc        0.0100
# The following items are used to identify the programs used.
_computing_cell_refinement       'RIETAN-FP (Izumi and Momma, 2007)'
_computing_structure_solution    'EXPO-2009 (Altomare et al., 2009)'
_computing_structure_refinement  'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics    'VESTA (Momma and Izumi, 2008)'
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
Zn1 0.6110(6) 0.2451(3) 0.1154(7) 1 8 c Uiso 0.0120(4) Zn
Zn2 0.6058(6) 0.2463(3) 0.2901(7) 1 8 c Uiso 0.0120 Zn
Zn3 0.5 0.5 0.4533 1 4 a Uiso 0.0120 Zn
K1 0.6607(9) 0.1614(4) 0.4914(8) 1 8 c Uiso 0.073(2) K
P1 0.8494(4) 0.3460(2) 0.2100(8) 1 8 c Uiso 0.0143(8) P
P2 0.632(1) 0.6196(7) 0.0685(8) 1 8 c Uiso 0.0143 P
P3 0.627(1) 0.6235(7) 0.3450(8) 1 8 c Uiso 0.0143 P
O1 0.751(2) 0.187(1) 0.0616(9) 1 8 c Uiso 0.0076(9) O
O2 0.536(2) 0.341(1) 0.0726(10) 1 8 c Uiso 0.0076 O
O3 0.441(1) 0.1664(9) 0.1437(8) 1 8 c Uiso 0.0076 O
O4 0.7040(7) 0.2864(4) 0.2036(9) 1 8 c Uiso 0.0076 O
O5 0.439(1) 0.1724(9) 0.2708(8) 1 8 c Uiso 0.0076 O
O6 0.537(2) 0.346(1) 0.338(1) 1 8 c Uiso 0.0076 O
O7 0.755(2) 0.194(1) 0.351(1) 1 8 c Uiso 0.0076 O
O8 0.635(1) 0.565(1) 0.403(1) 1 8 c Uiso 0.0076 O
O9 0.638(1) 0.562(1) 1.009(1) 1 8 c Uiso 0.0076 O
C1 0.7807(9) 0.4490(6) 0.208(1) 1 8 c Uiso 0.006(2) C
C2 0.679(2) 0.5692(7) 0.145(1) 1 8 c Uiso 0.006 C
C3 0.662(2) 0.5664(6) 0.268(1) 1 8 c Uiso 0.006 C
C4 0.6341(8) 0.6058(4) 0.206(1) 1 8 c Uiso 0.006 C
C5 0.754(2) 0.4904(8) 0.146(1) 1 8 c Uiso 0.006 C
C6 0.736(2) 0.4874(7) 0.269(1) 1 8 c Uiso 0.006 C
H1 0.569(2) 0.651(1) 0.2043(9) 1 8 c Uiso 0.006 H
H2 0.811(6) 0.473(2) 0.108(1) 1 8 c Uiso 0.006 H
H3 0.769(14) 0.466(8) 0.311(4) 1 8 c Uiso 0.006 H
Ow1 0.130(2) 0.6400(9) 0.423(1) 1 8 c Uiso 0.089 O
Ow2 0 0.5 0.4205(8) 1 4 b Uiso 0.089 O
#===============================================================================
#10. GEOMETRICAL PARAMETERS
_geom_special_details            ?
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
Zn1 O1 1.86(1) . 1_555 ?
Zn1 O2 1.88(1) . 1_555 ?
Zn1 O3 2.00(1) . 1_555 ?
Zn1 O4 2.04(1) . 1_555 ?
Zn2 O5 1.89(1) . 1_555 ?
Zn2 O7 1.94(1) . 1_555 ?
Zn2 O6 1.96(1) . 1_555 ?
Zn2 O4 2.02(1) . 1_555 ?
Zn3 O8 1.85(1) . 1_555 ?
Zn3 O9 1.90(1) . 7_564 ?
P1 O5 1.46(1) . 3_555 ?
P1 O3 1.55(1) . 3_555 ?
P1 O4 1.571(6) . 1_555 ?
P1 C1 1.768(9) . 1_555 ?
P2 O1 1.48(1) . 4_655 ?
P2 O9 1.50(1) . 1_554 ?
P2 O2 1.57(1) . 2_665 ?
P2 C2 1.78(2) . 1_555 ?
P3 O8 1.49(1) . 1_555 ?
P3 O6 1.49(1) . 2_665 ?
P3 O7 1.52(1) . 4_655 ?
P3 C3 1.81(2) . 1_555 ?
C1 C6 1.415(7) . 1_555 ?
C1 C5 1.422(6) . 1_555 ?
C2 C4 1.388(7) . 1_555 ?
C2 C5 1.426(6) . 1_555 ?
C3 C4 1.415(6) . 1_555 ?
C3 C6 1.423(6) . 1_555 ?
C4 H1 0.92(1) . 1_555 ?
C5 H2 0.94(1) . 1_555 ?
C6 H3 0.94(2) . 1_555 ?
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
O1 Zn1 O2 112.1(8) 1_555 . 1_555 ?
O1 Zn1 O3 107.3(7) 1_555 . 1_555 ?
O1 Zn1 O4 114.6(2) 1_555 . 1_555 ?
O2 Zn1 O3 114.1(6) 1_555 . 1_555 ?
O2 Zn1 O4 104.5(7) 1_555 . 1_555 ?
O3 Zn1 O4 104.3(1) 1_555 . 1_555 ?
O6 Zn2 O7 104.4(7) 1_555 . 1_555 ?
O6 Zn2 O5 113.1(6) 1_555 . 1_555 ?
O6 Zn2 O4 106.1(6) 1_555 . 1_555 ?
O7 Zn2 O5 109.7(7) 1_555 . 1_555 ?
O7 Zn2 O4 113.6(5) 1_555 . 1_555 ?
O5 Zn2 O4 109.9(4) 1_555 . 1_555 ?
O8 Zn3 O8 114(2) 1_555 . 2_665 ?
O8 Zn3 O9 103.9(1) 1_555 . 7_564 ?
O8 Zn3 O9 113.3(3) 1_555 . 8_654 ?
O9 Zn3 O9 108(1) 7_564 . 8_654 ?
O3 P1 O5 114.7(1) 3_555 . 3_555 ?
O3 P1 O4 104.3(2) 3_555 . 1_555 ?
O3 P1 C1 105.7(8) 3_555 . 1_555 ?
O5 P1 O4 110.6(6) 3_555 . 1_555 ?
O5 P1 C1 112.5(8) 3_555 . 1_555 ?
O4 P1 C1 108.5(4) 1_555 . 1_555 ?
O1 P2 O9 111(1) 4_655 . 1_554 ?
O1 P2 O2 109(1) 4_655 . 2_665 ?
O1 P2 C2 105(1) 4_655 . 1_555 ?
O9 P2 O2 108.8(9) 1_554 . 2_665 ?
O9 P2 C2 113(1) 1_554 . 1_555 ?
O2 P2 C2 110.2(5) 2_665 . 1_555 ?
O7 P3 O8 113(1) 4_655 . 1_555 ?
O7 P3 O6 112(1) 4_655 . 2_665 ?
O7 P3 C3 110(1) 4_655 . 1_555 ?
O8 P3 O6 109(1) 1_555 . 2_665 ?
O8 P3 C3 109(1) 1_555 . 1_555 ?
O6 P3 C3 104.3(2) 2_665 . 1_555 ?
P2 O1 Zn1 139(1) 4_645 . 1_555 ?
P2 O2 Zn1 132(1) 2_665 . 1_555 ?
P1 O3 Zn1 133.2(7) 3_455 . 1_555 ?
P1 O4 Zn1 125.2(7) 1_555 . 1_555 ?
P1 O4 Zn2 116.9(7) 1_555 . 1_555 ?
Zn1 O4 Zn2 117.9(3) 1_555 . 1_555 ?
P1 O5 Zn2 133.3(8) 3_455 . 1_555 ?
P3 O6 Zn2 127(1) 2_665 . 1_555 ?
P3 O7 Zn2 135(1) 4_645 . 1_555 ?
P3 O8 Zn3 139.1(4) 1_555 . 1_555 ?
P2 O9 Zn3 140.1(2) 1_556 . 7_565 ?
C6 C1 C5 119.7(8) 1_555 . 1_555 ?
C6 C1 P1 119.0(2) 1_555 . 1_555 ?
C5 C1 P1 121.0(9) 1_555 . 1_555 ?
C4 C2 C5 119.9(3) 1_555 . 1_555 ?
C4 C2 P2 118.9(2) 1_555 . 1_555 ?
C5 C2 P2 121.1(3) 1_555 . 1_555 ?
C4 C3 C6 119.5(3) 1_555 . 1_555 ?
C4 C3 P3 118.9(2) 1_555 . 1_555 ?
C6 C3 P3 121.1(2) 1_555 . 1_555 ?
H1 C4 C2 119(1) 1_555 . 1_555 ?
H1 C4 C3 119(1) 1_555 . 1_555 ?
C2 C4 C3 121.1(2) 1_555 . 1_555 ?
H2 C5 C2 119(1) 1_555 . 1_555 ?
H2 C5 C1 119(1) 1_555 . 1_555 ?
C2 C5 C1 119.8(7) 1_555 . 1_555 ?
H3 C6 C3 119(9) 1_555 . 1_555 ?
H3 C6 C1 120(8) 1_555 . 1_555 ?
C3 C6 C1 120.0(6) 1_555 . 1_555 ?


data_ZBP-Rb
_database_code_depnum_ccdc_archive 'CCDC 916296'
#TrackingRef 'web_deposit_cif_file_0_KazuyukiMaeda_1355832349.ZBPs_submission3.cif'
# 5. CHEMICAL DATA
_chemical_name_common            ZBP-Rb
_chemical_formula_moiety         'C12 H6 O20.44 P6 Rb2 Zn5'
_chemical_formula_sum            'C12 H10.88 O20.44 P6 Rb2 Zn5'
_chemical_formula_weight         1165.882
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn -0.3771 2.5535 'International Tables for Crystallography, Vol. C'
Rb Rb -1.5162 0.7344 'International Tables for Crystallography, Vol. C'
P P 0.1621 0.1866 'International Tables for Crystallography, Vol. C'
O O 0.0196 0.0127 'International Tables for Crystallography, Vol. C'
C C 0.0064 0.0035 'International Tables for Crystallography, Vol. C'
H H 0.0000 0.0000 'International Tables for Crystallography, Vol. C'
# 6. POWDER SPECIMEN AND CRYSTAL DATA
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_Int_Tables_number      56
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x+1/2,-y+1/2,z
3 -x,y+1/2,-z+1/2
4 x+1/2,-y,-z+1/2
5 -x,-y,-z
6 x+1/2,y+1/2,-z
7 x,-y+1/2,z+1/2
8 -x+1/2,y,z+1/2
_cell_length_a                   16.1861(4)
_cell_length_b                   8.5394(2)
_cell_length_c                   20.0976(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2777.9(1)
_cell_formula_units_Z            4
_exptl_crystal_density_diffrn    2.7877
_exptl_crystal_F_000             2241.78
_pd_spec_mounting                'Lindemann glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_colour                  colorless
# 7. EXPERIMENTAL DATA
_diffrn_ambient_temperature      300
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  Debye-Scherrer
_diffrn_detector                 'imaging plate'
_pd_meas_scan_method             fixed
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.99752
_pd_meas_number_of_points        7001
_pd_meas_2theta_range_min        3.0000
_pd_meas_2theta_range_max        73.0000
_pd_meas_2theta_range_inc        0.0100
# 8. REFINEMENT DATA
_pd_proc_ls_special_details      
; Anisotropic line broadening factors Ue and Pe were refined.
;
_pd_calc_method                  'Rietveld Refinement'
_pd_proc_ls_profile_function     'split pseudo-Voigt function'
_pd_proc_ls_background_function  'Legendre polynomials'
_pd_proc_ls_pref_orient_corr     
; ?
;
#; $P_k = \sum_{j=1}^{m_k} \frac{1}{m_k}
#\left( r^2 \cos^2 \alpha_j +r^{-1}\ sin^2 \alpha_j \right)^{-3/2}$
#with a preferred-orientation vector, (hkl),
#and <i>r</i> = 1.0(0)
_pd_proc_ls_prof_R_factor        0.00595
_pd_proc_ls_prof_wR_factor       0.00763
_pd_proc_ls_prof_wR_expected     0.00440
_refine_ls_R_I_factor            0.01745
_refine_ls_R_Fsqd_factor         0.01348
_refine_ls_R_factor_all          0.01224
_refine_special_details          
; A virtual chemical species Ow (1O and 2H) is introduced
for Ow1 and Ow2 to simulate water molecules.
;
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/<i>y</i>~i~
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_parameters     111
_refine_ls_number_restraints     97
_refine_ls_number_constraints    29
# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   1.7324
_refine_ls_shift/su_max          0.0
#_refine_diff_density_max 0.0
#_refine_diff_density_min 0.0
# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.
_pd_proc_2theta_range_min        4.5000
_pd_proc_2theta_range_max        55.0000
_pd_proc_2theta_range_inc        0.0100
# The following items are used to identify the programs used.
_computing_cell_refinement       'RIETAN-FP (Izumi and Momma, 2007)'
_computing_structure_solution    'EXPO-2009 (Altomare et al., 2009)'
_computing_structure_refinement  'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics    'VESTA (Momma and Izumi, 2008)'
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
Zn1 0.5026(3) 0.3566(6) 0.1633(4) 1 8 e Uiso 0.0168(6) Zn
Zn2 0.5076(3) 0.3549(6) 0.3363(4) 1 8 e Uiso 0.0168 Zn
Zn3 0.25 0.25 0 1 4 c Uiso 0.0168 Zn
P1 0.5938(2) 0.0948(4) 0.2464(7) 1 8 e Uiso 0.012(1) P
P2 0.3704(6) 0.122(1) 0.1087(6) 1 8 e Uiso 0.012 P
P3 0.3708(6) 0.112(1) 0.3846(6) 1 8 e Uiso 0.012 P
O1 0.5358(5) -0.0543(8) 0.2500(9) 1 8 e Uiso 0.0072(9) O
O2 0.4202(9) 0.680(2) 0.3199(9) 1 8 e Uiso 0.0072 O
O3 0.417(1) 0.696(2) 0.1927(7) 1 8 e Uiso 0.0072 O
O4 0.405(1) 0.295(2) 0.1169(9) 1 8 e Uiso 0.0072 O
O5 0.444(1) 0.005(2) 0.1023(8) 1 8 e Uiso 0.0072 O
O6 0.311(1) 0.110(2) 0.0543(10) 1 8 e Uiso 0.0072 O
O7 0.563(1) 0.494(2) 0.1073(8) 1 8 e Uiso 0.0072 O
O8 0.413(1) 0.266(2) 0.383(1) 1 8 e Uiso 0.0072 O
O9 0.313(1) 0.116(2) 0.445(1) 1 8 e Uiso 0.0072 O
C1 0.3000(5) 0.522(1) 0.2473(7) 1 8 e Uiso 0.0072 C
C2 0.2630(8) 0.483(2) 0.1838(7) 1 8 e Uiso 0.0072 C
C3 0.3177(8) 0.085(2) 0.1834(7) 1 8 e Uiso 0.0072 C
C4 0.1432(6) 0.380(1) 0.2447(8) 1 8 e Uiso 0.0072 C
C5 0.1823(6) 0.415(2) 0.3068(7) 1 8 e Uiso 0.0072 C
C6 0.2536(7) 0.503(2) 0.3063(8) 1 8 e Uiso 0.0072 C
H1 0.289(5) 0.512(15) 0.142(1) 1 8 e Uiso 0.0072 H
H2 0.099(2) 0.306(5) 0.2445(9) 1 8 e Uiso 0.0072 H
H3 0.278(3) 0.533(10) 0.348(1) 1 8 e Uiso 0.0072 H
Rb1 0.3970(4) 0.8998(9) 0.5344(4) 0.722(5) 8 e Uiso 0.067(2) Rb
Rb2 0.4115(6) 0.610(1) 0.4637(7) 0.278 8 e Uiso 0.067 Rb
Ow1 0.4115 0.610 0.4637 0.722 8 e Uiso 0.0287(9) O
Ow2 0.25 0.75 0.4651(7) 1 4 d Uiso 0.0287 O
#===============================================================================
#10. GEOMETRICAL PARAMETERS
_geom_special_details            ?
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
Zn1 O7 1.90(2) . 1_555 ?
Zn1 O4 1.91(1) . 1_555 ?
Zn1 O2 1.99(1) . 3_645 ?
Zn1 O1 2.00(1) . 3_655 ?
Zn2 O3 1.92(1) . 3_645 ?
Zn2 O5 1.95(2) . 3_655 ?
Zn2 O8 1.96(2) . 1_555 ?
Zn2 O1 2.02(2) . 3_655 ?
Zn3 O9 1.89(2) . 7_554 ?
Zn3 O6 1.90(1) . 1_555 ?
P1 O3 1.51(2) . 3_645 ?
P1 O2 1.53(2) . 3_645 ?
P1 O1 1.584(8) . 1_555 ?
P1 C1 1.832(8) . 3_645 ?
P2 O6 1.46(2) . 1_555 ?
P2 O5 1.56(1) . 1_555 ?
P2 O4 1.58(1) . 1_555 ?
P2 C3 1.76(1) . 1_555 ?
P3 O7 1.48(1) . 3_645 ?
P3 O8 1.48(1) . 1_555 ?
P3 O9 1.54(2) . 1_555 ?
P3 C5 1.80(1) . 2_555 ?
C1 C6 1.41(1) . 1_555 ?
C1 C2 1.45(1) . 1_555 ?
C2 H1 0.97(2) . 1_555 ?
C3 C4 1.42(1) . 2_555 ?
C3 C2 1.43(1) . 2_555 ?
C4 H2 0.96(2) . 1_555 ?
C5 C6 1.38(1) . 1_555 ?
C5 C4 1.43(1) . 1_555 ?
C6 H3 0.96(2) . 1_555 ?
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
O7 Zn1 O4 108.0(8) 1_555 . 1_555 ?
O7 Zn1 O1 116.1(4) 1_555 . 3_655 ?
O7 Zn1 O2 104.4(6) 1_555 . 3_645 ?
O4 Zn1 O1 105.8(7) 1_555 . 3_655 ?
O4 Zn1 O2 113.2(7) 1_555 . 3_645 ?
O1 Zn1 O2 109.5(6) 3_655 . 3_645 ?
O5 Zn2 O8 105.6(8) 3_655 . 1_555 ?
O5 Zn2 O3 113.7(7) 3_655 . 3_645 ?
O5 Zn2 O1 115.6(4) 3_655 . 3_655 ?
O8 Zn2 O3 111.7(8) 1_555 . 3_645 ?
O8 Zn2 O1 106.7(7) 1_555 . 3_655 ?
O3 Zn2 O1 103.4(4) 3_645 . 3_655 ?
O9 Zn3 O9 109(1) 7_554 . 8_554 ?
O9 Zn3 O6 116.0(3) 7_554 . 1_555 ?
O9 Zn3 O6 103.3(3) 7_554 . 2_555 ?
O6 Zn3 O6 110(1) 1_555 . 2_555 ?
O1 P1 O3 111(1) 1_555 . 3_645 ?
O1 P1 O2 109(1) 1_555 . 3_645 ?
O1 P1 C1 106.3(5) 1_555 . 3_645 ?
O3 P1 O2 114.7(4) 3_645 . 3_645 ?
O3 P1 C1 104.4(6) 3_645 . 3_645 ?
O2 P1 C1 111.1(7) 3_645 . 3_645 ?
O6 P2 O5 113(1) 1_555 . 1_555 ?
O6 P2 C3 108(1) 1_555 . 1_555 ?
O6 P2 O4 112(1) 1_555 . 1_555 ?
O5 P2 C3 109(1) 1_555 . 1_555 ?
O5 P2 O4 110(1) 1_555 . 1_555 ?
C3 P2 O4 104.4(6) 1_555 . 1_555 ?
C5 P3 O7 111(1) 2_555 . 3_645 ?
C5 P3 O9 114(1) 2_555 . 1_555 ?
C5 P3 O8 108.3(9) 2_555 . 1_555 ?
O7 P3 O9 112(1) 3_645 . 1_555 ?
O7 P3 O8 106(1) 3_645 . 1_555 ?
O9 P3 O8 106(1) 1_555 . 1_555 ?
P1 O1 Zn1 122(1) 1_555 . 3_645 ?
P1 O1 Zn2 118(1) 1_555 . 3_645 ?
Zn1 O1 Zn2 119.5(4) 3_645 . 3_645 ?
P1 O2 Zn1 126.9(9) 3_655 . 3_655 ?
P1 O3 Zn2 136.7(8) 3_655 . 3_655 ?
Zn1 O4 P2 127(1) 1_555 . 1_555 ?
P2 O5 Zn2 133(1) 1_555 . 3_645 ?
P2 O6 Zn3 137(1) 1_555 . 1_555 ?
P3 O7 Zn1 137(1) 3_655 . 1_555 ?
P3 O8 Zn2 136(1) 1_555 . 1_555 ?
Zn3 O9 P3 143(1) 7_555 . 1_555 ?
C6 C1 C2 119.5(5) 1_555 . 1_555 ?
C6 C1 P1 118.7(5) 1_555 . 3_655 ?
C2 C1 P1 121.8(4) 1_555 . 3_655 ?
H1 C2 C1 121(1) 1_555 . 1_555 ?
H1 C2 C3 120(2) 1_555 . 2_555 ?
C1 C2 C3 118.4(4) 1_555 . 2_555 ?
C2 C3 C4 119.4(7) 2_555 . 2_555 ?
C2 C3 P2 121.5(4) 2_555 . 1_555 ?
C4 C3 P2 119.1(8) 2_555 . 1_555 ?
H2 C4 C5 118(1) 1_555 . 1_555 ?
H2 C4 C3 118(1) 1_555 . 2_555 ?
C5 C4 C3 121.0(6) 1_555 . 2_555 ?
P3 C5 C4 121.4(4) 2_555 . 1_555 ?
P3 C5 C6 118.4(4) 2_555 . 1_555 ?
C4 C5 C6 118.6(4) 1_555 . 1_555 ?
H3 C6 C1 119(1) 1_555 . 1_555 ?
H3 C6 C5 119(1) 1_555 . 1_555 ?
C1 C6 C5 121.0(6) 1_555 . 1_555 ?


data_ZBP-Cs
_database_code_depnum_ccdc_archive 'CCDC 916297'
#TrackingRef 'web_deposit_cif_file_0_KazuyukiMaeda_1355832349.ZBPs_submission3.cif'
# 5. CHEMICAL DATA
_chemical_name_common            ZBP-Cs
_chemical_formula_moiety         'C12 H6 Cs2 O19.22 P6 Zn5'
_chemical_formula_sum            'C12 H8.44 Cs2 O19.22 P6 Zn5'
_chemical_formula_weight         1238.649
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn -0.3771 2.5535 'International Tables for Crystallography, Vol. C'
Cs Cs -0.2753 3.8219 'International Tables for Crystallography, Vol. C'
P P 0.1621 0.1866 'International Tables for Crystallography, Vol. C'
O O 0.0196 0.0127 'International Tables for Crystallography, Vol. C'
C C 0.0064 0.0035 'International Tables for Crystallography, Vol. C'
H H 0.0000 0.0000 'International Tables for Crystallography, Vol. C'
# 6. POWDER SPECIMEN AND CRYSTAL DATA
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_Int_Tables_number      60
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x+1/2,-y+1/2,z+1/2
3 -x,y,-z+1/2
4 x+1/2,-y+1/2,-z
5 -x,-y,-z
6 x+1/2,y+1/2,-z+1/2
7 x,-y,z+1/2
8 -x+1/2,y+1/2,z
_cell_length_a                   16.1877(3)
_cell_length_b                   8.5356(2)
_cell_length_c                   20.2585(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2799.1(1)
_cell_formula_units_Z            4
_exptl_crystal_density_diffrn    2.9392
_exptl_crystal_F_000             2336.69
_pd_spec_mounting                'Lindemann glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_colour                  colorless
# 7. EXPERIMENTAL DATA
_diffrn_ambient_temperature      300
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  Debye-Scherrer
_diffrn_detector                 'imaging plate'
_pd_meas_scan_method             fixed
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.99752
_pd_meas_number_of_points        7101
_pd_meas_2theta_range_min        3.00
_pd_meas_2theta_range_max        74.00
_pd_meas_2theta_range_inc        0.01
# 8. REFINEMENT DATA
_pd_proc_ls_special_details      
; Anisotropic line broadening factors Ue and Pe were refined.
;
_pd_calc_method                  'Rietveld Refinement'
_pd_proc_ls_profile_function     'split pseudo-Voigt function'
_pd_proc_ls_background_function  'Legendre polynomials'
_pd_proc_ls_pref_orient_corr     
; ?
;
#; $P_k = \sum_{j=1}^{m_k} \frac{1}{m_k}
#\left( r^2 \cos^2 \alpha_j +r^{-1}\ sin^2 \alpha_j \right)^{-3/2}$
#with a preferred-orientation vector, (hkl),
#and <i>r</i> = 1.0(0)
_pd_proc_ls_prof_R_factor        0.00869
_pd_proc_ls_prof_wR_factor       0.01145
_pd_proc_ls_prof_wR_expected     0.00627
_refine_ls_R_I_factor            0.01912
_refine_ls_R_Fsqd_factor         0.01233
_refine_ls_R_factor_all          0.01138
_refine_special_details          
; A virtual chemical species Ow (1O and 2H) is introduced
for Ow1 and Ow2 to simulate water molecules.
;
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/<i>y</i>~i~
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_parameters     117
_refine_ls_number_restraints     97
_refine_ls_number_constraints    24
# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   1.8267
_refine_ls_shift/su_max          0.0
#_refine_diff_density_max 0.0
#_refine_diff_density_min 0.0
# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.
_pd_proc_2theta_range_min        4.5000
_pd_proc_2theta_range_max        65.0000
_pd_proc_2theta_range_inc        0.0100
# The following items are used to identify the programs used.
_computing_cell_refinement       'RIETAN-FP (Izumi and Momma, 2007)'
_computing_structure_solution    'EXPO-2009 (Altomare et al., 2009)'
_computing_structure_refinement  'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics    'VESTA (Momma and Izumi, 2008)'
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
Zn1 0.2460(2) 0.6056(5) 0.0826(2) 1 8 d Uiso 0.0185(5) Zn
Zn2 0.7562(2) 0.3968(5) 0.0885(1) 1 8 d Uiso 0.0185 Zn
Zn3 0.5 0.4966(5) 0.25 1 4 c Uiso 0.0185 Zn
P1 0.6174(4) 0.6268(9) 0.1354(3) 1 8 d Uiso 0.0102(8) P
P2 0.3800(4) 0.3585(8) 0.1372(2) 1 8 d Uiso 0.0102 P
P3 0.1562(2) 0.3439(4) -0.0020(3) 1 8 d Uiso 0.0102 P
O1 0.1902(7) 0.746(1) 0.1420(5) 1 8 d Uiso 0.0088(8) O
O2 0.3385(8) 0.519(1) 0.1317(5) 1 8 d Uiso 0.0088 O
O3 0.1737(7) 0.436(1) 0.0583(4) 1 8 d Uiso 0.0088 O
O4 0.2825(4) 0.6970(6) 0.0001(6) 1 8 d Uiso 0.0088 O
O5 0.8173(8) 0.258(1) 0.1432(5) 1 8 d Uiso 0.0088 O
O6 0.6570(7) 0.466(1) 0.1302(5) 1 8 d Uiso 0.0088 O
O7 0.8324(7) 0.561(1) 0.0668(4) 1 8 d Uiso 0.0088 O
O8 0.4365(6) 0.3591(9) 0.1958(5) 1 8 d Uiso 0.0088 O
O9 0.5595(6) 0.632(1) 0.1941(5) 1 8 d Uiso 0.0088 O
C1 0.4460(4) 0.7754(9) 0.0004(4) 1 8 d Uiso 0.004(2) C
C2 0.5643(6) 0.668(2) 0.0604(5) 1 8 d Uiso 0.004 C
C3 0.4335(7) 0.321(2) 0.0582(4) 1 8 d Uiso 0.004 C
C4 0.6037(5) 0.641(1) 0.0017(5) 1 8 d Uiso 0.004 C
C5 0.4852(7) 0.738(2) 0.0614(5) 1 8 d Uiso 0.004 C
C6 0.5124(9) 0.252(2) 0.0594(6) 1 8 d Uiso 0.004 C
H1 0.652(2) 0.576(4) 0.0015(6) 1 8 d Uiso 0.004 H
H2 0.453(2) 0.742(15) 0.101(1) 1 8 d Uiso 0.004 H
H3 0.538(4) 0.223(13) 0.1002(8) 1 8 d Uiso 0.004 H
Cs1 0.3506(2) 0.8760(3) 0.2156(1) 0.802(1) 8 d Uiso 0.0636(7) Cs
Cs2 0.1526(6) 0.625(1) 0.2862(5) 0.198 8 d Uiso 0.0636 Cs
Ow1 0.019(1) 0.521(2) 0.2904(6) 0.5 8 d Uiso 0.0352(8) O
Ow2 0.25 0.125 0.197(4) 0.109(8) 8 d Uiso 0.0352 O
#===============================================================================
#10. GEOMETRICAL PARAMETERS
_geom_special_details            ?
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
Zn1 O1 1.92(1) . 1_555 ?
Zn1 O3 1.93(1) . 1_555 ?
Zn1 O4 1.94(1) . 1_555 ?
Zn1 O2 1.94(1) . 1_555 ?
Zn2 O5 1.90(1) . 1_555 ?
Zn2 O6 1.91(1) . 1_555 ?
Zn2 O7 1.92(1) . 1_555 ?
Zn2 O4 2.06(1) . 5_665 ?
Zn3 O9 1.883(8) . 1_555 ?
Zn3 O8 1.908(8) . 1_555 ?
P1 O9 1.517(8) . 1_555 ?
P1 O6 1.52(1) . 1_555 ?
P1 O5 1.55(1) . 8_655 ?
P1 C2 1.78(1) . 1_555 ?
P2 O1 1.49(1) . 8_545 ?
P2 O8 1.498(7) . 1_555 ?
P2 O2 1.53(1) . 1_555 ?
P2 C3 1.846(8) . 1_555 ?
P3 O3 1.479(8) . 1_555 ?
P3 O7 1.555(7) . 5_665 ?
P3 O4 1.600(6) . 8_545 ?
P3 C1 1.756(7) . 8_545 ?
C1 C6 1.41(1) . 5_665 ?
C1 C5 1.424(8) . 1_555 ?
C2 C4 1.368(9) . 1_555 ?
C2 C5 1.41(1) . 1_555 ?
C3 C4 1.39(1) . 5_665 ?
C3 C6 1.41(2) . 1_555 ?
C4 H1 0.95(1) . 1_555 ?
C5 H2 0.96(1) . 1_555 ?
C6 H3 0.96(1) . 1_555 ?
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
O2 Zn1 O1 106.2(5) 1_555 . 1_555 ?
O2 Zn1 O3 108.1(4) 1_555 . 1_555 ?
O2 Zn1 O4 111.1(4) 1_555 . 1_555 ?
O1 Zn1 O3 110.0(5) 1_555 . 1_555 ?
O1 Zn1 O4 115.6(2) 1_555 . 1_555 ?
O3 Zn1 O4 105.6(4) 1_555 . 1_555 ?
O6 Zn2 O5 111.9(5) 1_555 . 1_555 ?
O6 Zn2 O7 114.7(3) 1_555 . 1_555 ?
O6 Zn2 O4 104.4(3) 1_555 . 5_665 ?
O5 Zn2 O7 104.7(5) 1_555 . 1_555 ?
O5 Zn2 O4 115.1(2) 1_555 . 5_665 ?
O7 Zn2 O4 106.2(4) 1_555 . 5_665 ?
O8 Zn3 O9 107.9(2) 1_555 . 1_555 ?
O8 Zn3 O8 104.1(2) 1_555 . 3_655 ?
O8 Zn3 O9 116.6(2) 1_555 . 3_655 ?
O9 Zn3 O9 104.2(3) 1_555 . 3_655 ?
O5 P1 O9 108.6(6) 8_655 . 1_555 ?
O5 P1 O6 112.0(6) 8_655 . 1_555 ?
O5 P1 C2 105.9(8) 8_655 . 1_555 ?
O9 P1 O6 110.0(7) 1_555 . 1_555 ?
O9 P1 C2 111.4(6) 1_555 . 1_555 ?
O6 P1 C2 108.9(6) 1_555 . 1_555 ?
O1 P2 O8 114.6(3) 8_545 . 1_555 ?
O1 P2 O2 104.3(3) 8_545 . 1_555 ?
O1 P2 C3 107.6(8) 8_545 . 1_555 ?
O8 P2 O2 108.9(7) 1_555 . 1_555 ?
O8 P2 C3 113.6(6) 1_555 . 1_555 ?
O2 P2 C3 107.2(6) 1_555 . 1_555 ?
O3 P3 O7 113.4(5) 1_555 . 5_665 ?
O3 P3 O4 105.9(7) 1_555 . 8_545 ?
O3 P3 C1 109.5(6) 1_555 . 8_545 ?
O7 P3 O4 111.0(7) 5_665 . 8_545 ?
O7 P3 C1 108.1(5) 5_665 . 8_545 ?
O4 P3 C1 108.9(4) 8_545 . 8_545 ?
P2 O1 Zn1 136.0(7) 8_555 . 1_555 ?
P2 O2 Zn1 135.8(7) 1_555 . 1_555 ?
P3 O3 Zn1 136.5(8) 1_555 . 1_555 ?
P3 O4 Zn1 121.9(8) 8_555 . 1_555 ?
P3 O4 Zn2 118.0(8) 8_555 . 5_665 ?
Zn1 O4 Zn2 120.1(3) 1_555 . 5_665 ?
P1 O5 Zn2 138.3(7) 8_645 . 1_555 ?
P1 O6 Zn2 131.7(7) 1_555 . 1_555 ?
P3 O7 Zn2 130.8(7) 5_665 . 1_555 ?
P2 O8 Zn3 141.9(4) 1_555 . 1_555 ?
P1 O9 Zn3 140.3(5) 1_555 . 1_555 ?
C5 C1 C6 119.8(5) 1_555 . 5_665 ?
C5 C1 P3 121.2(3) 1_555 . 8_555 ?
C6 C1 P3 118.9(4) 5_665 . 8_555 ?
C4 C2 C5 120.3(5) 1_555 . 1_555 ?
C4 C2 P1 118.9(4) 1_555 . 1_555 ?
C5 C2 P1 120.6(5) 1_555 . 1_555 ?
C4 C3 C6 120.2(5) 5_665 . 1_555 ?
C4 C3 P2 121.0(6) 5_665 . 1_555 ?
C6 C3 P2 118.9(3) 1_555 . 1_555 ?
H1 C4 C2 119(1) 1_555 . 1_555 ?
H1 C4 C3 119(1) 1_555 . 5_665 ?
C2 C4 C3 121.3(4) 1_555 . 5_665 ?
H2 C5 C1 119(1) 1_555 . 1_555 ?
H2 C5 C2 121(2) 1_555 . 1_555 ?
C1 C5 C2 119.0(5) 1_555 . 1_555 ?
H3 C6 C1 120(1) 1_555 . 5_665 ?
H3 C6 C3 121(1) 1_555 . 1_555 ?
C1 C6 C3 119.4(6) 5_665 . 1_555 ?


data_ZBP-NH4
_database_code_depnum_ccdc_archive 'CCDC 916298'
#TrackingRef 'web_deposit_cif_file_0_KazuyukiMaeda_1355832349.ZBPs_submission3.cif'
# 5. CHEMICAL DATA
_chemical_name_common            ZBP-NH4
_chemical_formula_moiety         'C12 H6 N2 O21 P6 Zn5'
_chemical_formula_sum            'C12 H18 N2 O21 P6 Zn5'
_chemical_formula_weight         1039.015
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn -0.3771 2.5535 'International Tables for Crystallography, Vol. C'
P P 0.1621 0.1866 'International Tables for Crystallography, Vol. C'
O O 0.0196 0.0127 'International Tables for Crystallography, Vol. C'
N N 0.0115 0.0070 'International Tables for Crystallography, Vol. C'
C C 0.0064 0.0035 'International Tables for Crystallography, Vol. C'
H H 0.0000 0.0000 'International Tables for Crystallography, Vol. C'
# 6. POWDER SPECIMEN AND CRYSTAL DATA
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'I b a 2'
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_Int_Tables_number      45
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,z
3 x+1/2,-y+1/2,z
4 -x+1/2,y+1/2,z
5 x+1/2,y+1/2,z+1/2
6 -x+1/2,-y+1/2,z+1/2
7 x,-y,z+1/2
8 -x,y,z+1/2
_cell_length_a                   8.5337(2)
_cell_length_b                   16.1764(3)
_cell_length_c                   19.9903(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2759.5(1)
_cell_formula_units_Z            4
_exptl_crystal_density_diffrn    2.5009
_exptl_crystal_F_000             2048.00
_pd_spec_mounting                'Lindemann glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_colour                  colorless
# 7. EXPERIMENTAL DATA
_diffrn_ambient_temperature      300
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  Debye-Scherrer
_diffrn_detector                 'imaging plate'
_pd_meas_scan_method             fixed
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.99860
_pd_meas_number_of_points        7101
_pd_meas_2theta_range_min        3.00
_pd_meas_2theta_range_max        74.00
_pd_meas_2theta_range_inc        0.01
# 8. REFINEMENT DATA
_pd_proc_ls_special_details      
; Anisotropic line broadening factors Ue and Pe were refined.
;
_pd_calc_method                  'Rietveld Refinement'
_pd_proc_ls_profile_function     'split pseudo-Voigt function'
_pd_proc_ls_background_function  'Legendre polynomials'
_pd_proc_ls_pref_orient_corr     
; ?
;
#; $P_k = \sum_{j=1}^{m_k} \frac{1}{m_k}
#\left( r^2 \cos^2 \alpha_j +r^{-1}\ sin^2 \alpha_j \right)^{-3/2}$
#with a preferred-orientation vector, (hkl),
#and <i>r</i> = 1.0(0)
_pd_proc_ls_prof_R_factor        0.00570
_pd_proc_ls_prof_wR_factor       0.00749
_pd_proc_ls_prof_wR_expected     0.01085
_refine_ls_R_I_factor            0.01958
_refine_ls_R_Fsqd_factor         0.01357
_refine_ls_R_factor_all          0.01220
_refine_special_details          
; Virtual chemical species Ow (1O and 2H) for Ow1 and Ow2
and Nh (1N and 3H) for Nh1 are introduced to simulate
water and ammonia molecules.
;
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/<i>y</i>~i~
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_parameters     111
_refine_ls_number_restraints     97
_refine_ls_number_constraints    20
# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   0.6908
_refine_ls_shift/su_max          0.0
#_refine_diff_density_max 0.0
#_refine_diff_density_min 0.0
# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.
_pd_proc_2theta_range_min        4.5000
_pd_proc_2theta_range_max        65.0000
_pd_proc_2theta_range_inc        0.0100
# The following items are used to identify the programs used.
_computing_cell_refinement       'RIETAN-FP (Izumi and Momma, 2007)'
_computing_structure_solution    'EXPO-2009 (Altomare et al., 2009)'
_computing_structure_refinement  'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics    'VESTA (Momma and Izumi, 2008)'
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
Zn1 0.6102(7) 0.2480(4) 0.117(4) 1 8 c Uiso 0.0108(6) Zn
Zn2 0.6027(7) 0.2430(4) 0.292(4) 1 8 c Uiso 0.0108 Zn
Zn3 0.5 0.5 0.453(4) 1 4 a Uiso 0.0108 Zn
P1 0.8437(5) 0.3428(3) 0.207(4) 1 8 c Uiso 0.014(1) P
P2 0.624(1) 0.6211(9) 0.068(4) 1 8 c Uiso 0.014 P
P3 0.641(1) 0.620(1) 0.344(4) 1 8 c Uiso 0.014 P
O1 0.763(2) 0.194(1) 0.063(4) 1 8 c Uiso 0.002(1) O
O2 0.540(2) 0.349(1) 0.077(4) 1 8 c Uiso 0.002 O
O3 0.430(3) 0.173(1) 0.141(4) 1 8 c Uiso 0.002 O
O4 0.6989(9) 0.2837(5) 0.207(4) 1 8 c Uiso 0.002 O
O5 0.441(3) 0.165(1) 0.268(4) 1 8 c Uiso 0.002 O
O6 0.528(2) 0.337(1) 0.341(4) 1 8 c Uiso 0.002 O
O7 0.737(2) 0.185(1) 0.348(4) 1 8 c Uiso 0.002 O
O8 0.647(2) 0.563(1) 0.401(4) 1 8 c Uiso 0.002 O
O9 0.633(2) 0.563(1) 1.009(4) 1 8 c Uiso 0.002 O
C1 0.772(1) 0.4467(6) 0.206(5) 1 8 c Uiso 0.005(3) C
C2 0.664(2) 0.566(1) 0.145(5) 1 8 c Uiso 0.005 C
C3 0.679(2) 0.568(1) 0.265(4) 1 8 c Uiso 0.005 C
C4 0.637(1) 0.6049(5) 0.205(5) 1 8 c Uiso 0.005 C
C5 0.730(2) 0.487(1) 0.144(4) 1 8 c Uiso 0.005 C
C6 0.748(2) 0.488(1) 0.265(5) 1 8 c Uiso 0.005 C
H1 0.576(4) 0.651(2) 0.205(5) 1 8 c Uiso 0.005 H
H2 0.725(17) 0.457(3) 0.107(5) 1 8 c Uiso 0.005 H
H3 0.800(8) 0.471(2) 0.302(5) 1 8 c Uiso 0.005 H
Nh1 0.655(3) 0.166(2) 0.500(4) 1 8 c Uiso 0.127 N
Ow1 0 0.5 0.416(4) 1 4 b Uiso 0.076 O
Ow2 0.126(3) 0.642(1) 0.427(4) 1 8 c Uiso 0.076 O
#===============================================================================
#10. GEOMETRICAL PARAMETERS
_geom_special_details            ?
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
Zn1 O2 1.91(2) . 1_555 ?
Zn1 O1 1.91(2) . 1_555 ?
Zn1 O3 2.02(2) . 1_555 ?
Zn1 O4 2.03(2) . 1_555 ?
Zn2 O7 1.86(2) . 1_555 ?
Zn2 O6 1.92(3) . 1_555 ?
Zn2 O5 1.93(2) . 1_555 ?
Zn2 O4 1.99(2) . 1_555 ?
Zn3 O9 1.90(2) . 7_564 ?
Zn3 O8 1.93(2) . 1_555 ?
P1 O5 1.48(2) . 3_555 ?
P1 O3 1.53(2) . 3_555 ?
P1 O4 1.563(8) . 1_555 ?
P1 C1 1.786(9) . 1_555 ?
P2 O2 1.49(2) . 2_665 ?
P2 O9 1.51(2) . 1_554 ?
P2 O1 1.52(2) . 4_655 ?
P2 C2 1.80(3) . 1_555 ?
P3 O8 1.47(2) . 1_555 ?
P3 O7 1.48(2) . 4_655 ?
P3 O6 1.60(2) . 2_665 ?
P3 C3 1.82(3) . 1_555 ?
C1 C6 1.38(2) . 1_555 ?
C1 C5 1.45(2) . 1_555 ?
C2 C4 1.37(2) . 1_555 ?
C2 C5 1.40(2) . 1_555 ?
C3 C4 1.38(2) . 1_555 ?
C3 C6 1.42(2) . 1_555 ?
C4 H1 0.91(3) . 1_555 ?
C5 H2 0.88(3) . 1_555 ?
C6 H3 0.91(3) . 1_555 ?
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
O1 Zn1 O2 112(1) 1_555 . 1_555 ?
O1 Zn1 O3 112(1) 1_555 . 1_555 ?
O1 Zn1 O4 112.3(7) 1_555 . 1_555 ?
O2 Zn1 O3 112(1) 1_555 . 1_555 ?
O2 Zn1 O4 104(1) 1_555 . 1_555 ?
O3 Zn1 O4 104(1) 1_555 . 1_555 ?
O6 Zn2 O7 107.4(9) 1_555 . 1_555 ?
O6 Zn2 O5 114(1) 1_555 . 1_555 ?
O6 Zn2 O4 108.0(7) 1_555 . 1_555 ?
O7 Zn2 O5 105(1) 1_555 . 1_555 ?
O7 Zn2 O4 115(1) 1_555 . 1_555 ?
O5 Zn2 O4 107.8(6) 1_555 . 1_555 ?
O8 Zn3 O8 114.8(6) 1_555 . 2_665 ?
O8 Zn3 O9 102(1) 1_555 . 7_564 ?
O8 Zn3 O9 115(1) 1_555 . 8_654 ?
O9 Zn3 O9 107.4(9) 7_564 . 8_654 ?
O3 P1 O5 115.3(4) 3_555 . 3_555 ?
O3 P1 O4 106(2) 3_555 . 1_555 ?
O3 P1 C1 108(1) 3_555 . 1_555 ?
O5 P1 O4 113(2) 3_555 . 1_555 ?
O5 P1 C1 106(1) 3_555 . 1_555 ?
O4 P1 C1 107.8(5) 1_555 . 1_555 ?
O1 P2 O9 113(1) 4_655 . 1_554 ?
O1 P2 O2 110(2) 4_655 . 2_665 ?
O1 P2 C2 109(1) 4_655 . 1_555 ?
O9 P2 O2 110(1) 1_554 . 2_665 ?
O9 P2 C2 110(1) 1_554 . 1_555 ?
O2 P2 C2 103.6(4) 2_665 . 1_555 ?
O7 P3 O8 111(1) 4_655 . 1_555 ?
O7 P3 O6 109(1) 4_655 . 2_665 ?
O7 P3 C3 104.4(8) 4_655 . 1_555 ?
O8 P3 O6 110(1) 1_555 . 2_665 ?
O8 P3 C3 113(1) 1_555 . 1_555 ?
O6 P3 C3 109.3(8) 2_665 . 1_555 ?
P2 O1 Zn1 138(1) 4_645 . 1_555 ?
P2 O2 Zn1 129(2) 2_665 . 1_555 ?
P1 O3 Zn1 132(1) 3_455 . 1_555 ?
P1 O4 Zn1 118(2) 1_555 . 1_555 ?
P1 O4 Zn2 122(2) 1_555 . 1_555 ?
Zn1 O4 Zn2 120(1) 1_555 . 1_555 ?
P1 O5 Zn2 131(1) 3_455 . 1_555 ?
P3 O6 Zn2 132(2) 2_665 . 1_555 ?
P3 O7 Zn2 139(1) 4_645 . 1_555 ?
P3 O8 Zn3 136.6(9) 1_555 . 1_555 ?
P2 O9 Zn3 140.2(7) 1_556 . 7_565 ?
C6 C1 C5 119(1) 1_555 . 1_555 ?
C6 C1 P1 120(1) 1_555 . 1_555 ?
C5 C1 P1 121(1) 1_555 . 1_555 ?
C4 C2 C5 120(1) 1_555 . 1_555 ?
C4 C2 P2 119(1) 1_555 . 1_555 ?
C5 C2 P2 121(1) 1_555 . 1_555 ?
C4 C3 C6 121(1) 1_555 . 1_555 ?
C4 C3 P3 121(1) 1_555 . 1_555 ?
C6 C3 P3 119(1) 1_555 . 1_555 ?
H1 C4 C2 119(1) 1_555 . 1_555 ?
H1 C4 C3 119(1) 1_555 . 1_555 ?
C2 C4 C3 121(1) 1_555 . 1_555 ?
H2 C5 C2 120(3) 1_555 . 1_555 ?
H2 C5 C1 119(1) 1_555 . 1_555 ?
C2 C5 C1 120(1) 1_555 . 1_555 ?
H3 C6 C3 119(1) 1_555 . 1_555 ?
H3 C6 C1 119(1) 1_555 . 1_555 ?
C3 C6 C1 120(1) 1_555 . 1_555 ?
#===END