Synthesis, Characterization, and Properties of Organically Templated Lanthanide Oxalatophosphates with a Three-Dimensional Honeycomb Structure: (H4APPIP)[Ln3(C2O4)5.5(H2PO4)2].5H2O (Ln = Er-Lu, APPIP = 1,4-Bis(3-aminopropyl)piperazine)
Chih-Min Wang; Yi-Ying Wu; Chia-Hung Hou; Chii-Chang Chen; Kwang-Hwa Lii; Inorganic Chemistry 48 (2009) 1519–1523; doi:10.1021/ic801817e

data_4301458
_publ_contact_author
;
Kwang-Hwa Lii
Department of Chemistry
National Central University
Jhongli, Taiwan 320
;
_publ_contact_author_email
;
liikh@cc.ncu.edu.tw
;
_publ_section_title
;
Synthesis, Characterization, and Properties of Organically Templated
Lanthanide Oxalatophosphates with a Three-Dimensional Honeycomb Structure:
(H4APPIP)[Ln3(C2O4)5.5(H2PO4)2].5H2O (Ln = Er-Lu, APPIP =
1,4-Bis(3-aminopropyl)piperazine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1519
_journal_page_last               1523
_journal_paper_doi               10.1021/ic801817e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C21 H42 Er3 N4 O35 P2'
_chemical_formula_weight         1474.31
_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                 96.212(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5146(2)
_cell_length_b                   16.2049(5)
_cell_length_c                   28.5470(8)
_cell_measurement_temperature    293(2)
_cell_volume                     3915.74(19)
_computing_cell_refinement       'SHELXTL software'
_computing_data_collection       'SHELXTL software'
_computing_data_reduction        'SHELXTL software'
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega scan'
_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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            39815
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    6.579
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS program'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.501
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         8956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+5.4530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                6821
_reflns_number_total             8956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801817e_si_002.cif
_cod_data_source_block           i8019_0m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301458