[Zn3(HPO4)4](NMe4)2: a zincophosphate containing interruptions of isolated hydrogen-bonding [H–O(P)]4 groupings within a novel three-dimensional four-connected framework
Wiebcke, Michael; Journal of Materials Chemistry 12 (2002) 421–; doi:10.1039/b106274n

data_7204217
_publ_section_title
;
 [Zn3(HPO4)4](NMe4)2: a zincophosphate containing interruptions of
 isolated hydrogen-bonding [H--O(P)]4 groupings within a novel
 three-dimensional four-connected framework
;
_journal_issue                   3
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              421
_journal_paper_doi               10.1039/b106274n
_journal_volume                  12
_journal_year                    2002
_chemical_formula_sum            'C8 H28 N2 O16 P4 Zn3'
_chemical_formula_weight         728.32
_chemical_name_systematic
;
Bis-tetramethylammonium-tri-zinc-tetra-hydrogenphosphate
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   'geom difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2001-10-18T20:08:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.203(1)
_cell_length_b                   15.776(2)
_cell_length_c                   31.587(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      14.54
_cell_measurement_theta_min      10.49
_cell_volume                     4586.0(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       \w/2\Q-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            3519
_diffrn_reflns_theta_full        29.95
_diffrn_reflns_theta_max         29.95
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    3.469
_exptl_absorpt_correction_T_max  0.4980
_exptl_absorpt_correction_T_min  0.4198
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1668
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0330P)^2^+10.5839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                1040
_reflns_number_total             1668
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106274n.txt
_cod_data_source_block           I
_cod_original_cell_volume        4586(1)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7204217
_exptl_absorpt_correction_t_ave  0.4508