Synthesis of open-framework zinc phosphates from organophosphorus amides
Neeraj, S.; Cheetham, A. K.; Chemical Communications  (2002) 1738–; doi:10.1039/b205557k

data_7114161
_publ_section_title
;
 Synthesis of open-framework zinc phosphates from organophosphorus amides
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1738
_journal_paper_doi               10.1039/b205557k
_journal_year                    2002
_chemical_formula_moiety         '[(C2NH8)(H3O)][Zn4(PO4)3(H2O)]2.H2O'
_chemical_formula_sum            'C H4 N0.5 O14 P3 Zn4'
_chemical_formula_weight         601.44
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           34
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.284(3)
_cell_length_b                   17.726(3)
_cell_length_c                   5.1882(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1405.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_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  0.1247
_diffrn_reflns_av_sigmaI/netI    0.1002
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            8025
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    7.157
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.842
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Long needles'
_exptl_crystal_F_000             1162
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.456
_refine_diff_density_rms         0.266
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3174
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1121P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.1813
_reflns_number_gt                2593
_reflns_number_total             3174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205557k.txt
_cod_data_source_block           Compound_II
_cod_original_formula_sum        'C H4 N0.50 O14 P3 Zn4'
_cod_database_code               7114161