#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:53:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179311 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/08/4320874.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320874
loop_
_publ_author_name
'Yun-Ling Liu'
'Guang-Shan Zhu'
'Jie-Sheng Chen'
'Li-Yan Na'
'Jia Hua'
'Wen-Qin Pang'
'Ru-Ren Xu'
_publ_section_title
;
 Synthesis and Structural Characterization of a New Open-Framework Tin(II)
 Phosphate: [Sn4(PO4)3]-.0.5[C4N2H12]2+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1820
_journal_page_last               1822
_journal_paper_doi               10.1021/ic991241e
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C2 H6 N O12 P3 Sn4'
_chemical_formula_weight         803.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.341(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0884(16)
_cell_length_b                   23.336(4)
_cell_length_c                   9.0429(18)
_cell_measurement_reflns_used    137
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.24
_cell_measurement_theta_min      2.3
_cell_volume                     1455.5(5)
_computing_cell_refinement       'Bruker SMART '
_computing_data_collection       'Bruker SMART '
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2921
_diffrn_reflns_theta_full        23.24
_diffrn_reflns_theta_max         23.24
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    7.175
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.991
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0366P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                1750
_reflns_number_total             1997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991241e.cif
_cod_data_source_block           '[Sn4(PO4)3]-.0.5[C4N2H12]2+'
_cod_database_code               4320874
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Sn1 Sn 0.23910(7) 0.24205(2) 0.40660(6) 0.01966(17) Uani 1 1 d . . .
Sn2 Sn 0.24365(8) 0.42215(3) 0.06401(6) 0.02081(17) Uani 1 1 d . . .
Sn3 Sn 0.35586(8) 0.66684(2) 0.25768(6) 0.01965(17) Uani 1 1 d . . .
Sn4 Sn 0.20392(8) 0.85196(2) 0.23694(6) 0.01813(17) Uani 1 1 d . . .
P1 P 0.4168(3) 0.36945(9) 0.4044(2) 0.0166(4) Uani 1 1 d . . .
P2 P 0.2314(3) 0.56163(9) 0.0160(2) 0.0172(5) Uani 1 1 d . . .
P3 P 0.0844(3) 0.74503(9) 0.4154(2) 0.0165(4) Uani 1 1 d . . .
O1 O 0.2712(8) 0.3310(2) 0.4585(6) 0.0228(13) Uani 1 1 d . . .
O2 O 0.3149(8) 0.4200(2) 0.3081(6) 0.0261(13) Uani 1 1 d . . .
O3 O 0.3314(8) 0.5072(3) 0.0895(6) 0.0319(15) Uani 1 1 d . . .
O4 O 0.0375(7) 0.5485(2) -0.0971(6) 0.0213(12) Uani 1 1 d . . .
O5 O 0.3626(7) 0.5937(2) -0.0678(6) 0.0225(13) Uani 1 1 d . . .
O6 O 0.1849(8) 0.6000(2) 0.1442(6) 0.0241(13) Uani 1 1 d . . .
O7 O 0.4409(7) 0.6058(2) 0.4557(5) 0.0198(12) Uani 1 1 d . . .
O8 O 0.1264(8) 0.6844(2) 0.3652(6) 0.0214(12) Uani 1 1 d . . .
O9 O 0.0656(7) 0.7447(2) 0.5822(5) 0.0200(12) Uani 1 1 d . . .
O10 O -0.1142(7) 0.7667(2) 0.3233(5) 0.0211(13) Uani 1 1 d . . .
O11 O 0.2486(7) 0.7858(2) 0.3998(6) 0.0227(13) Uani 1 1 d . . .
O12 O 0.4777(8) 0.8330(2) 0.1925(5) 0.0222(13) Uani 1 1 d . . .
N1 N 0.1495(11) 0.5198(3) 0.4308(8) 0.037(2) Uani 1 1 d . . .
H1A H 0.2409 0.5460 0.4257 0.080 Uiso 1 1 calc . . .
H1B H 0.1526 0.4926 0.3608 0.080 Uiso 1 1 calc . . .
C2 C -0.0409(14) 0.5473(4) 0.3967(10) 0.035(2) Uani 1 1 d . . .
H2A H -0.0699 0.5614 0.2931 0.080 Uiso 1 1 calc . . .
H2B H -0.0392 0.5797 0.4640 0.080 Uiso 1 1 calc . . .
C1 C 0.1938(14) 0.4934(4) 0.5844(10) 0.036(2) Uani 1 1 d . . .
H1C H 0.3168 0.4734 0.6006 0.080 Uiso 1 1 calc . . .
H1D H 0.2062 0.5234 0.6604 0.080 Uiso 1 1 calc . . .
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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 Sn1 O10 87.2(2) . 2_545 ?
O1 Sn1 O9 84.8(2) . 3_566 ?
O10 Sn1 O9 79.47(19) 2_545 3_566 ?
O3 Sn2 O2 85.1(2) . . ?
O3 Sn2 O4 86.8(2) . 3_565 ?
O2 Sn2 O4 82.7(2) . 3_565 ?
O6 Sn3 O8 87.1(2) . . ?
O6 Sn3 O7 86.4(2) . . ?
O8 Sn3 O7 81.41(19) . . ?
O11 Sn4 O12 89.0(2) . . ?
O11 Sn4 O5 84.1(2) . 4_576 ?
O12 Sn4 O5 87.27(19) . 4_576 ?
O1 P1 O12 108.1(3) . 2_645 ?
O1 P1 O7 108.7(3) . 3_666 ?
O12 P1 O7 111.4(3) 2_645 3_666 ?
O1 P1 O2 111.5(3) . . ?
O12 P1 O2 109.1(3) 2_645 . ?
O7 P1 O2 108.1(3) 3_666 . ?
O5 P2 O3 110.4(3) . . ?
O5 P2 O4 108.6(3) . . ?
O3 P2 O4 112.1(3) . . ?
O5 P2 O6 110.2(3) . . ?
O3 P2 O6 108.1(3) . . ?
O4 P2 O6 107.4(3) . . ?
O11 P3 O8 110.0(3) . . ?
O11 P3 O9 109.3(3) . . ?
O8 P3 O9 110.5(3) . . ?
O11 P3 O10 111.3(3) . . ?
O8 P3 O10 110.9(3) . . ?
O9 P3 O10 104.7(3) . . ?
P1 O1 Sn1 123.2(3) . . ?
P1 O2 Sn2 124.5(3) . . ?
P2 O3 Sn2 130.4(3) . . ?
P2 O4 Sn2 123.1(3) . 3_565 ?
P2 O5 Sn4 114.5(3) . 4_575 ?
P2 O6 Sn3 126.5(3) . . ?
P1 O7 Sn3 114.8(3) 3_666 . ?
P3 O8 Sn3 122.4(3) . . ?
P3 O9 Sn1 110.5(3) . 3_566 ?
P3 O10 Sn1 123.7(3) . 2 ?
P3 O11 Sn4 121.6(3) . . ?
P1 O12 Sn4 125.6(3) 2_655 . ?
C2 N1 C1 111.4(7) . . ?
C2 N1 H1A 109.4 . . ?
C1 N1 H1A 109.4 . . ?
C2 N1 H1B 109.4 . . ?
C1 N1 H1B 109.4 . . ?
H1A N1 H1B 108.0 . . ?
N1 C2 C1 111.1(8) . 3_566 ?
N1 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 3_566 . ?
N1 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 3_566 . ?
H2A C2 H2B 108.0 . . ?
C2 C1 N1 111.8(7) 3_566 . ?
C2 C1 H1C 109.3 3_566 . ?
N1 C1 H1C 109.3 . . ?
C2 C1 H1D 109.3 3_566 . ?
N1 C1 H1D 109.3 . . ?
H1C C1 H1D 107.9 . . ?
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
Sn1 O1 2.128(6) . ?
Sn1 O10 2.142(5) 2_545 ?
Sn1 O9 2.207(5) 3_566 ?
Sn2 O3 2.077(6) . ?
Sn2 O2 2.148(5) . ?
Sn2 O4 2.192(5) 3_565 ?
Sn3 O6 2.093(5) . ?
Sn3 O8 2.118(5) . ?
Sn3 O7 2.259(5) . ?
Sn4 O11 2.106(5) . ?
Sn4 O12 2.117(5) . ?
Sn4 O5 2.253(5) 4_576 ?
P1 O1 1.532(6) . ?
P1 O12 1.534(5) 2_645 ?
P1 O7 1.538(5) 3_666 ?
P1 O2 1.543(6) . ?
P2 O5 1.525(6) . ?
P2 O3 1.529(6) . ?
P2 O4 1.543(5) . ?
P2 O6 1.558(6) . ?
P3 O11 1.535(6) . ?
P3 O8 1.537(6) . ?
P3 O9 1.545(5) . ?
P3 O10 1.546(5) . ?
O4 Sn2 2.192(5) 3_565 ?
O5 Sn4 2.253(5) 4_575 ?
O7 P1 1.538(5) 3_666 ?
O9 Sn1 2.207(5) 3_566 ?
O10 Sn1 2.142(5) 2 ?
O12 P1 1.534(5) 2_655 ?
N1 C2 1.461(12) . ?
N1 C1 1.485(12) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
C2 C1 1.480(13) 3_566 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C1 C2 1.480(13) 3_566 ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O7 0.90 1.96 2.851(9) 169.0 .
N1 H1B O2 0.90 2.16 2.938(10) 143.9 .
