Synthesis and Structural Characterization of a New Open-Framework Tin(II) Phosphate: [Sn4(PO4)3]-.0.5[C4N2H12]2+
Yun-Ling Liu; Guang-Shan Zhu; Jie-Sheng Chen; Li-Yan Na; Jia Hua; Wen-Qin Pang; Ru-Ren Xu; Inorganic Chemistry 39 (2000) 1820–1822; doi:10.1021/ic991241e

data_4320874
_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/[\s^2^(Fo^2^)+(0.0366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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